Table of Contents Index - Cromlab...2007/12/28 · POROS Becton, Dickinson and Company Luer-LOK Bio-Rad Laboratories, Inc. Aminex Biotage AB EVOLUTE, Isolute Bristol-Myers Squibb

Index

i

Table of Contents

Column Selection

SPE Phase Selection ...........................................................2HPLC and LC/MS Column Selection ...................................4GC Column Selection ........................................................17

SPE

HyperSep SPE Products ....................................................30 Finnpipettes.......................................................................46

GC and GC/MS

TRACE GC Capillary Columns ...........................................48 Ultra Fast GC Columns......................................................65

HPLC and LC/MS

Column Protection.............................................................66Hypersil GOLD Columns....................................................70 BioBasic Columns..............................................................88 Hypercarb Columns .........................................................101 Hypersil BDS Columns ....................................................106 Hypersil Classical Columns.............................................111 Polymeric HPLC Columns ................................................122 AQUASIL C18 Columns ...................................................128 BetaBasic Columns .........................................................129 BetaMax Columns...........................................................130 BETASIL Columns ............................................................130 Other HPLC Columns .......................................................132

Accessories for HPLC and GC

HPLC Accessories............................................................136HPLC Injectors and Valves ..............................................144 GC Accessories ...............................................................150 Syringes...........................................................................161 Vials, Caps and Vial Accessories....................................169

Chromatography and Mass SpectrometryInstrument Parts and Supplies

GC and GC/MS................................................................176

Turboflow Columns..........................................................188

LC and LC/MS .................................................................189

MS ...............................................................................195

IRMS ...............................................................................198

ICP-MS ............................................................................199

Technical Information

SPE Method Development and Troubleshooting............204 HPLC Method Selection, Troubleshooting

and Reference Data...............................................207 GC Method Selection, Troubleshooting

and Reference Data...............................................221

Applications

Pharma/Biochem.............................................................230 Environmental .................................................................258 Forensics/Toxicology .......................................................276 Industrial .........................................................................288 Food Safety .....................................................................302

Indexes

Applications Index...........................................................318 Alphabetical Index ..........................................................330

317

229

203

175

135

47

65

29

1

Trademark Information

The Thermo Scientific name, the Thermo Scientific logo and the following trademarks are the property of Thermo Fisher Scientific Inc. and/or its subsidiaries:

Trademark Information

To order or for customer support, please see back cover.ii

3M CompanyKel-F

Agilent Technologies, Inc.AccuBOND, Agilent, DB, Evidex, HP-INNOWax, HP-Ultra, Zorbax

Applera CorporationPOROS

Becton, Dickinson and CompanyLuer-LOK

Bio-Rad Laboratories, Inc.Aminex

Biotage ABEVOLUTE, Isolute

Bristol-Myers Squibb CompanyTaxol

Capital Analytical, Ltd.RH

Chromatography Research Supplies, Inc.BTO

Cohesive Technologies, Inc.Aria

Dow Chemical Company, TheTRITON X-100

E.I. Dupont de Nemours and CompanyTeflon, Tefzel, Vespel, Viton

Eka Chemicals ABKromasil

Floridin CompanyFlorisil

General Electric CompanySE

GL Sciences, Inc.Inertsil

Hamilton CompanyHamilton

HighChem, Ltd.Mass Frontier

Hewlett-Packard Development CompanyHP

Kimberly-Clark CorporationKimwipes

Macherey-Nagel GmbHCHROMABOND, NUCLEODUR, Nucleosil, Optima

Mallinckrodt Baker, Inc.BAKERBOND spe, BAKERBOND, Polar Plus

Merck KGaALiChrosorb, LiChrospher, Purospher

Merlin Instrument CompanyMicroseal

Neos CorporationFluofix

New Objective, Inc.IntegraFrit, PicoFrit

Ohio Valley Specialty Chemical CompanyOV

Parker Hannifin CorporationParker

PerkinElmer, Inc.Clarus , PE

Pfizer, Inc.Dostinex

Phenomenex, Inc.AQUA, Columbus, Gemini, Jupiter, Luna, Prodigy,strata, Synergi, Ultracarb, Zebron ZB

Porvair plcPorvair

Quadrex Corporation007

Restek CorporationRtx, Stabilwax, Pinnacle, Viva

Rheodyne LLCMake-Before-Break (MBB), RheBuild, RheFlex,Rheodyne

Scientific Glass Technology Exploitatie B.V.CLICK-ON, Shortix, SGT, Super Clean

SGE, Inc.Auto-Sep T, Auto-Sep, BP, BPX, Enduro, SGE,PEEKsil, SilTite, Terry Tool

Shimadzu CorporationShimadzu

Showa Denko K.K.Asahipak, Shodex

Sigma-Aldrich CorporationDiscovery, Meridian MDN, Nukol, Petrocol, PTE, SP,SPB, SPME, Supelclean, Supelcosil, SUPELCOWAX,VOCOL

Tosoh CorporationTSKgel

Union Carbide CorporationCarbowax

United Chemical Technologies, Inc.Clean-Up

University of WashingtonSEQUEST, TurboSEQUEST

Upchurch Scientific, Inc.Bottom-of-the-Bottle, Upchurch Scientific

Varian, Inc.Bond Elut, Bond Elut Certify, CB, CC, CP-Select, CP-Sil, CP-Wax, Polaris, Pursuit, Varian

Velcro Industries B.V.Velcro

VICI, Valco Instruments Co., Inc.Cheminert, Valco

Victrex plc.VICTREX, PEEK

Waters CorporationµBondapak, ACQUITY UPLC, Atlantis, Nova-Pak,Sep-Pak, Styragel, SunFire, Symmetry, Ultrahydrogel,Ultrastyragel, Waters, µBondapak, Waters Spherisorb,Symmetry, SymmetryShield, XBridge, Xterra

Whatman, Inc.Partisil

W.R. Grace & CompanyAlltima, AT, Denali, Genesis, Vydac

YMC Co., Ltd.ODS-AQ, ODS-A, Pro-C18, YMCbasic, YMC-Pack,YMC

Other Notes:AquaSil™ Siliconizing Fluid for treating glass surfaces issold by Pierce Chemical Co., Rockford, IL

The following brands, trademarks or service marks are the property of the listed company and/or its subsidiaries.Every effort has been taken to ensure this list is accurate at the time of printing this catalog.

BetaBasic

BetaMax

BETASIL

BioBasic

BioMate

BioWorks

ChromQuest

COOL POCKET

DASH

Deca

DELTABOND

Discovery

DSQ

Dual Desolvation Zone

Evolution

Fingerlok

Finnigan

Fluophase

FocusLiner

FOCUS

HOT POCKET

Hypercarb

HyperGEL

Hypersil

Hypersil GOLD

Hypersil GOLD aQ

HyperPrep

HyperQuad

HyperREZ

HyperSep

HyPURITY

HyPURITY ADVANCE

HyPURITY AQUASTAR

Ion Bright

Javelin

KAPPA

LCQ

LCQ Advantage

LightPipe

LTQ

LTQ FT

LXQ

MSQ

Open Access

PRISM

ProteomeX

Retain

SLIPFREE

Smart Accessories

SpectraSYSTEM

Spectronic

Surveyor

Surveyor MSQ Plus

Surveyor Plus

TRACE

TRACE GC Ultra

Transcend

TriPlus

TSQ Quantum

TSQ Quantum Ultra

UNIGUARD

Verify

Watson LIMS

Xcalibur

Applications

ApplicationsCompiled from our years of experience in chromatography,

the Application Compendium contains HPLC, GC and SPE

applications to help you find the solution you need. For your

convenience, the applications are sorted by industry:

• Pharmaceutical/Biochemical, page 230• Environmental, page 258• Forensics/Toxicology, page 276• Industrial, page 288• Food Safety, page 302

Looking for data on a specific compound? Please refer to

the Applications Index on page 318. For more applications,

visit the Chromatography Resource Center at

www.thermo.com/columns.

Ibuprofen and Impurities Method Transfer from HPLC to U-HPLCThe modified European Pharmacopeia (EP) HPLC method for ibuprofen and related substances has been transferred to U-HPLC , reducing analysis time while maintaining chromatographic integrity.

Sub-2 µm particle packed columns offer advantages over the moretraditional columns packed with 3 and 5 µm particles by providingshorter analysis times, improvements in resolving power, sensitivityand peak capacity. When transferring methods from HPLC to U-HPLCif both particle size and column dimensions are also reduced, significantsavings in analysis time and solvent consumption can be achieved.However, care must be taken to ensure operating flow rate, gradientprofiles and injection volumes are scaled appropriately to obtain anequivalent or superior separation. This application note illustrates thesavings that can be made when transferring a method (adapted fromthe EP) from a 150 x 4.6 mm 5 µm column to a 50 x 2.1 mm columnpacked with 1.9 µm particles.

Experimental ConditionsOriginal HPLC Method

Instrument: Accela™ U-HPLC systemColumn: Hypersil GOLD™ 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: 0.05% H3PO4 in H2O/ACN (66:34)

B: ACN Gradient: Time (min) % B

0 025 055 8570 85

Flow Rate: 1.0 mL/minInjection Volume: 10 µLDetection: UV at 214 nm (0.1 s rise time; 20 Hz)Temperature: 30 °C

Fast U-HPLC Method

Instrument: Accela U-HPLC systemColumn: Hypersil GOLD 1.9 µm, 50 x 2.1 mmPart Number: 25002-052130Mobile Phase: A: 0.05% H3PO4 in H2O/ACN (66:34)

B: ACN Gradient: Time (min) % B

0 03.2 07.1 858.9 85

Flow Rate: 0.55 mL/minInjection Volume: 0.7 µLDetection: UV at 214 nm (0.1 s rise time; 20 Hz)Temperature: 30 °C

Results and DiscussionThe method was transferred geometrically to the 50 x 2.1 mm, 1.9 µmcolumn by scaling the flow rate, injection volume and gradient profile togive an equivalent separation in terms of chromatographic efficiency.The chromatographic profiles obtained for the original HPLC method (a)and the geometrically scaled U-HPLC method (b) are shown in the figure above. The resolution (USP) of peaks 5 and 6 is maintained (1.6)while analysis time is reduced by approximately seven-fold (last peakelutes at 46.5 min and 6.5 min, respectively). If column re-equilibrationtime between runs is taken into consideration then an eight-foldreduction in analysis time and a fourteen-fold reduction in solventconsumption were observed with the U-HPLC method.

References1. L. Pereira et al, Poster presented at Pittcon 2007, Chicago (reference PO20371_E 02/07)

Figure 1: Chromatograms obtained with the original HPLC and geometricallyscaled U-HPLC method.

(a)

(b)

H250-118

H250-121

Analytes: 1. Impurity K; 2. Impurity D; 3. Impurity C; 4. Ibuprofen; 5. Impurity A; 6. Impurity B; 7. Impurity E.

Pharma/Biochem

To order or for customer support, please see back cover.230

Porous Graphitic Carbon for the LC/MS Analysis of Hydrophilic PeptidesThe advantages of using porous graphitic carbon (PGC) in the LC/MS analysis of di-, tetra- andpenta-peptides containing polar and basic terminal amino acid residues are demonstrated.

Small hydrophilic peptides are not retained and, therefore, are oftenfound in the flow-through fraction from a C18 LC column, the type ofstationary phase most commonly used for the separation of proteolyticdigests of proteins. The analysis of the flow-through fraction requireseither a stationary phase that can retain the peptides away from thesolvent front, where the biological salts and buffers elute, or a sample clean-up step to remove the salts.1 PGC’s retention mechanisminvolves a charge-induced interaction of the polar analyte with thepolarizable surface of the graphite.2 PGC is an ideal stationary phaseideal to retain and resolve very polar, hydrophilic molecules, whichare normally not retained under reversed-phase LC using typical MScompatible mobile phases. In this application note it is demonstratedhow PGC columns increase capacity factors over alkyl-silica columnsfor small hydrophilic peptides.

Experimental Conditions

Instrument: Surveyor™ and LCQ™ DecaColumns: Hypercarb™ 5 µm, 50 x 2.1 mm

Hypersil GOLD 5 µm, 100 x 2.1 mmPart Numbers: 35005-052130 and 25005-102130Mobile Phase: A: H2O + 0.1% Formic acid

B: ACN + 0.1% Formic acidGradient: 5 to 100% B in 10 min Flow Rate: 0.2 mL/minInjection Volume: 10 µLDetection: + ESITemperature: 30 °C

Results and DiscussionIn the figure the retention of a di-, tetra- and a penta-peptide is com-pared on the alkyl-silica phase and on PGC. On the alkyl-silica phase,typically used in the separation of proteolytic digests, RGES elutes atthe solvent front, closely followed by DSDPR. The basic (Arg) andalcohol (Ser) terminal residues make these short peptides hydrophilicand difficult to retain under conventional reversed-phase LC/MS conditions. On the PGC column these short peptides are well retainedaway from the solvent front. PGC provides higher retention (capacityfactor) and different selectivity.

References1. E. T. Chin, D. I. Papac, Anal. Biochem. 273 (1999) pp 179 –1852. P. Ross, LCGC Europe, May 2000

Figure 1: Comparison of the retention of 3 hydrophilic peptides on alkyl-silica andporous graphitic carbon. PGC provides higher retention and different selectivity.

Analytes: 1. Arg-Gly-Glu-Ser (RGES); 2. Asp-Ser-Asp-Pro-Arg (DSDPR); 3. Gly-Tyr (GY)

(a) Alkyl-silica

NL: 4.15E7m/z = 447.7-448.7

NL: 2.17E7m/z = 447.7-448.7

NL: 3.92E7m/z = 294.6-295.6+

588.7-589.7

NL: 4.01E7m/z = 294.6-295.6+

588.7-589.7

NL: 2.73E7m/z = 238.5-239.5

NL: 4.69E7m/z = 238.5-239.5

NL: 4.16E7Base Peak

NL: 4.69E7Base Peak

PGC(b)

H250-123

H350-1133

Part Number:25005-102130

Part Number:35005-052130

Applications

www.thermo.com /columns 231

On-Line Sample Clean-Up for the LC/MS Analysis ofSmall Molecules in SerumOn-line sample clean-up utilizing SEC for the removal of matrix interferents from biologicalsamples reduces the total time required for analysis and has the added advantage of being easily automated.

Drug discovery/detection commonly focuses on analytes which arepresent in biological matrices. Direct injection of such samples ontoLC and LC/MS systems is problematic as analytes of interest can be‘lost’ in the concentrated matrix peak, plus instrument and columncontamination readily occurs. Traditionally, solid phase extraction (SPE)has been used for sample pre-treatment and clean-up, but this can betime consuming and adds an additional stage to the analytical method.

The ability to automate biological assays, minimize the numberof steps and reduce overall analysis time is becoming increasinglyimportant. On-line sample clean-up utilizing size exclusion chromatog-raphy (SEC) fulfills these criteria. On-line SEC is a two-dimensionalapproach in which serum is injected directly onto a small pore sizeexclusion column and then the analytes, once separated from thematrix, are eluted onto an analytical column. On-line SEC reducessample preparation time, minimizes potential analyte loss and resultsin increased productivity and higher sample throughput.1


Instrument: Surveyor™/LCQ™ Deca LC/MSColumns: BioBasic™ SEC-60 5 µm, 150 x 2.1 mm*

Hypersil GOLD™ 3 µm, 50 x 2.1 mmPart Numbers: 73305-152130 and 25003-052130 Mobile Phase: A: 10 mM ammonium formate, pH 3.0

B: MeOHGradient: Time (min) % B

0* 0 0.75 00.80 137.0 137.10 100

10.10 10010.20 1313.20 13

Flow Rate: 500 µL/minInjection Volume: 2 µLDetection: + ESITemperature: 45 °C

* SEC column equilibrated with 100% buffer for 2 min before start of gradient,eluent diverted to waste.

Results and DiscussionTo determine the time to divert the flow to waste after sample injec-tion, a comparison of the injections of serum alone and serum dosedwith the analyte was performed. Figure 1a shows the resultant UVtrace for blank serum. Lamivudine (the least retained of the analytes)was found to elute at ~ 0.8 minutes, therefore the switch valve wasset to direct flow to the analytical column at 0.75 minutes. The majorserum peak elutes earlier at ~ 0.5 minutes and, therefore, is preventedfrom contaminating the analytical column.

The separation of the drugs from serum with on-line SEC teamedwith isocratic analytical separation is depicted in Figure 1b. The percentage recoveries achieved were greater than 100, 89 and 79%for abacavir, lamivudine and zidovudine, respectively. During thecourse of experimentation, over 110 runs were performed with no significant deterioration in column performance observed, illustratingthat the methodology is robust and reproducible.

References1. C.E. Blythe et al, Poster presented at HPLC 2007, Ghent, Belgium. (Reference

PO20389_E06/07)

Figure 1: (a) Blank serum SEC extraction to determine valve switch time. (b) On-Line SEC Extraction of Anti-Retrovirals from Serum

Analytes: 1. Lamivudine; 2. Zidovudine; 3. Abacavir.

(a)K733-005

(b)

Pharma/Biochem


Applications


Pharmaceutical and Biochemical

Cyclosporin from BloodCompounds: CyclosporinPart Number: 60108-304Phase: HyperSep™ C18Volume: 3 mLBed Weight: 500 mgSample Mix 1 mL heparinised bloodPretreatment: with 2 mL water/acetonitrile

(7:3, v/v). Stir mixture and centrifuge after 5 min

Conditioning: 3 mL acetonitrile followed by 3 mLwater/acetonitrile (8:2, v/v)

Application: Force or aspirate the sampleslowly through column

Washing: 0.5 M acetic acid/acetonitrile (8:2, v/v) followed by 0.5 M acetic acid/acetonitrile (6:4, v/v)

Elution: Acetonitrile

Antineoplastic Agentsfrom PlasmaCompounds: Bisantrene, mitoxantronePart Number: 60108-302Phase: HyperSep C18Volume: 1 mLBed Weight: 100 mgConditioning: 2 mL methanol followed by 2 mL

distilled waterApplication: Force or aspirate 1-2 mL plasma

slowly through columnWashing: 2 mL distilled waterElution: 2 x 200 µL volumes 0.5 M

methanolic HCl

Antiarrhythmic DrugFlecainide from PlasmaCompounds: FlecainidePart Number: 60108-392Phase: HyperSep C8Volume: 1 mLBed Weight: 100 mgSample Mix 1 mL plasma with 1 mL waterPretreatment: and 200 µL 0.2 M sodium carbonate

solutionConditioning: 2 mL methanol followed by 2 mL

distilled waterApplication: Force or aspirate sample slowly

through columnWashing: 2 mL distilled waterElution: 500 µL methanol, then elute from

column after 1 min

Antiepileptics from SerumCompounds: Carbamazepine, dilantin,

phenobarbital, primidonePart Number: 60108-302Phase: HyperSep C18Volume: 1 mLBed Weight: 100 mgSample Mix 500 µL serum with 500 µL Pretreatment: 4-methylprimidone in citrate

buffer pH 4 (internal standard)Conditioning: 2 mL methanol followed by

2 mL waterApplication: Force or aspirate sample slowly

through columnWashing: 2 column volumes distilled waterElution: 2 x 100 µL volumes acetone

Gabapentin in Serum,Plasma or Whole BloodCompounds: GabapentinPart Number: 60108-302Phase: HyperSep C18Volume: 1 mLBed Weight: 100 mgSample 500 µL sample, calibrator or Pretreatment: control to be placed into a glass

test tube. Add 25 µL internal standard (5.0 mg/L). Add 500 µL20% acetic acid and vortex tube.

Conditioning: 3 mL CH3OH followed by 3 mL deionised water and 1 mL 100 mM HCl

Application: Load sample at 1-2 mL/minWashing: 3 mL deionized water followed by

3 mL ethyl acetate and 3 mLhexane. Dry column under vacuumfor 30 sec

Elution: 1 mL 2% NH4OH in CH3OHEvaporate to dryness at < 40 °C

Find more applications at the ChromatographyResource Center at www.thermo.com/columns.

CatecholamineMetabolites from UrineCompounds: Vanillylmandelic acid,

homovanillic acidPart Number: 60108-521Phase: HyperSep™ SAXVolume: 3 mLBed Weight: 500 mgSample Collect 24h urine (preservedPretreatment: with 0.1 M HCl). Store at 4 °C

Dilute sample prior to extraction1:1 with water. Use 0.5 M NaOHto adjust pH to 7.5.

Conditioning: 6 mL methanol followed by 6 mL distilled water

Application: Force or aspirate pretreated sample through column

Washing: 6 mL distilled waterElution: 6 mL 1.5 M sodium hydroxide

solution

Ketamine in UrineCompounds: KetaminePart Number: 60108-742Phase: HyperSep Verify™-CXVolume: 10 mLBed Weight: 200 mgSample To 2 mL urine add internal standardPretreatment: and 1 mL 100 mM phosphate

buffer (pH 6). Mix/vortex. Use 100 mM monobasic or dibasic sodium phosphate to ensure sample pH of 6

Conditioning: 3 mL CH3OH followed by 3 mL deionized water and 1 mL 100 mM phosphate buffer (pH 6)

Application: Load at 1 mL/minWashing: 3 mL deionized water

1 mL 100 mM acetic acid3 mL CH3OHDry column (5 min at > 10 inches Hg)

Elution: 3 mL dichloromethane/isopropanol/ammonium hydroxide (78:20:2) – collect eluents at 1-2 mL/min using minimal vacuumEvaporate to dryness at < 40 °C

Pharma/Biochem


BenadrylColumn: Hypersil GOLD™, 5 µm,

150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: 0.1% Formic acid

B: ACN Gradient: 5 to 100% B in 15 minFlow Rate: 1 mL/minDetection: UV at 254 nmTemperature: 25 °C

1. Benadryl

CS002-010

Column: Hypercarb™, 5 µm, 50 x 2.1 mmPart Number: 35005-052130Mobile Phase: A: H2O + 0.1% DEA

B: ACN:IPA (1:1)Gradient: 3 to 100% B in 10 minFlow Rate: 0.4 mL/minDetection: - ESI Temperature: 25 °C

1. 13-cis-Retinoic acid

2. 9-cis-Retinoic acid

Retinoic Acid IsomersH350-1004

0 4 8 12 MIN

1

1

2

Column: Hypersil GOLD, 5 µm, 150 x 4.6 mm

Part Number: 25005-154630Mobile Phase: A: 0.1% Formic acid

B: ACN + 0.1% Formic acidGradient: 35 to 70% B in 20 minFlow Rate: 1 mL/minDetection: UV at 254 nmTemperature: 25 °C

1. Cortisone2. 11-α-Hydroxyprogesterone3. 17-α-Hydroxyprogesterone4. Progesterone

SteroidsH250-012

Column: Hypercarb, 3 µm, 100 x 2.1 mmPart Number: 35003-102130Mobile Phase: A: 0.05% TFA

B: ACN + 0.05% TFAIsocratic: 70:30Flow Rate: 0.2 mL/minDetection: + ESITemperature: 40 °C

1. Isoniazid 2. Pyrazinamide

Tuberculostatics06010403

Applications


Column: HyPURITY AQUASTAR, 5 µm, 100 x 2.1 mm

Part Number: 22505-102130Mobile Phase: A: H2O + 0.1%

Heptafluorobutyric acidB: ACN + 0.1%

Heptafluorobutyric acidIsocratic: 50:50Flow Rate: 0.2 mL/minDetection: + ESI Temperature: 30 °C

1. Streptomycin

Streptomycin30040401

Column: HyPURITY AQUASTAR™, 5 µm, 100 x 2.1 mm




1. Tobramycin2. Neomycin

AminoglycosideAntibiotics

30040402

Column: HyPURITY AQUASTAR, 5 µm, 100 x 2.1 mm




1. Gentamicin C1a2. Gentamicin C23. Gentamicin C1

Gentamicin C Complex30040403

GoserelinColumn: Hypersil GOLD™, 5 µm,



1. Goserelin

CS002-009

1

2, 3

Pharma/Biochem


Column: Hypercarb™, 5 µm, 100 x 4.6 mmPart Number: 35005-104630Mobile Phase: A: ACN

B: 0.1% TFAIsocratic: 70:30Flow Rate: 1 mL/minDetection: UV at 254 nm

1. Uracil2. Prednisolone3. Dexamethasone4. Hydrocortisone

Steroids7032

Column: Hypercarb, 3 µm, 100 x 2.1 mmPart Number: 35003-102130Mobile Phase: A: H2O + 0.1% Formic acid

B: ACN + 0.1% Formic acidGradient: 30 to 100% B in 10 minFlow Rate: 0.2 mL/minDetection: + ESI Temperature: 40 °C

Acyclovir

Acyclovir12020402

Column: Hypercarb, 7 µm, 100 x 4.6 mmPart Number: 35007-104630Mobile Phase: 0.025 mM DCHT

(dicyclohexyltartrate)in KH2PO4 at pH 2.8

Flow Rate: 0.4 mL/minDetection: UV at 195 nmSource: C Petterson, Uppsala University,

Sweden

1. Scopolamine 4. (R)-Atropine2. (R)-Homatropine 5. (S)-Atropine3. (S)-Homatropine 6. Racemic Tropic Acid

Analogues of Atropine7052

Column: Hypercarb, 7 µm, 100 x 4.6 mmPart Number: 35007-104630Mobile Phase: A: MeOH

B: 0.025 M KH2PO4 at pH 4.5C: CH3COOH

Isocratic: 95:4.5:0.5Flow Rate: 1 mL/minDetection: UV at 240 nmSource: B. J. Clark, University

of Bradford, UK

1. 1-Methyl-4-nitro-5-chloroimidazole2. 6-Mercaptopurine3. Azathioprine

Antineoplastics7001



B: MeOH + 0.1% Formic acidGradient: 50 to 60% B in 20 minFlow Rate: 1 mL/minDetection: UV at 254 nmTemperature: 25 °C

1. Prednisone2. Prednisolone3. Hydrocortisone-21-acetate

SteroidsH250-011

Column: Hypersil GOLD™, 5 µm, 50 x 2.1 mmPart Number: 25005-052130Mobile Phase: A: 0.1% Formic acid


1. t02. Loperamide

LoperamideHydrochloride Tablet

H250-020

1

Applications


Column: Hypercarb™, 3 µm, 100 x 2.1 mmPart Number: 35003-102130Mobile Phase: A: 0.1% NH3 (aq)

B: ACN Isocratic: 90:10Flow Rate: 0.15 mL/minDetection: - ESITemperature: 30 °C

1. Fosfomycin (phosphomycin)

Fosfomycin01030402

Column: Hypercarb, 3 µm, 100 x 2.1 mmPart Number: 35003-102130Mobile Phase: A: 0.1% NH3 (aq)

B: ACN Isocratic: 50:50Flow Rate: 0.2 mL/minDetection: - ESI Temperature: 60 °C

1. Glucosamine sulfate

Glucosamine Sulfate01030401

Column: Hypercarb, 7 µm, 100 x 4.6 mmPart Number: 35007-104630Mobile Phase: 2.5 mM L-ZGP + 0.4 mM TEA in

CH2Cl2Flow Rate: 1 mL/minDetection: UV at 278 nmSource: Dr. C. Petterson, University of

Uppsala, Sweden

1. R-Metoprolol tartrate2. S-Metoprolol tartrate

Metoprolol Tartrate19070402


Part Number: 25005-154630Mobile Phase: A: 10 mM NH4COOH at pH 3.0

B: MeOHIsocratic: 20:80Flow Rate: 1 mL/minDetection: UV at 230 nmTemperature: 60 °C

1. Cyclosporin

Cyclosporin19050401

Column: Hypersil GOLD™, 5 µm, 150 x 4.6 mm

Part Number: 25005-154630Mobile Phase: A: 10 mM NaH2PO4 at pH 2.5

B: MeOH Isocratic: 65:35Flow Rate: 1 mL/minDetection: UV at 230 nmTemperature: 25 °C

1. Tablet component 4. Caffeine2. Codeine 5. Tablet component3. Acetaminophen

Analgesic TabletH250-013



B: MeOH + 0.1% Formic acidIsocratic: 70:30Flow Rate: 1 mL/minDetection: UV at 235 nmTemperature: 25 °C

1. Cloxazolam

Cloxazolam TabletH250-016

1 1

Pharma/Biochem



B: ACNIsocratic: 40:60Flow Rate: 1 mL/minDetection: UV at 280 nmTemperature: 40 °C

1. Estriol2. Estradiol3. Estrone

EstrogensH250-075

Column: Hypersil GOLD, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: 0.1% Acetic acid

B: ACNGradient: 20-70% B in 10 minFlow Rate: 1 mL/minDetection: UV at 254 nmTemperature: 25 °C

1. Cefadroxil2. Cefaclor3. Cephalexin4. Cephradine5. Cefazolin

Cepha AntibioticsH250-073

Column: Hypersil GOLD, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: 0.1% Formic acid

B: ACNGradient: 55-100% B in 5 minFlow Rate: 1 mL/minDetection: UV at 220 nmTemperature: 25 °C

1. Aspirin2. Piroxicam3. Sulindac4. Ibuprofen

Anti-Inflammatory/Analgesics

H250-074

Column: Hypersil GOLD, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: 20 mM NH4COOH, pH 3


1. Cyclizine2. Chlorocyclizine

AntihistaminesH250-078

Column: Hypersil GOLD, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: 20 mM NH4OAc pH 6

B: MeOHIsocratic: 60:40Flow Rate: 1.5 mL/minDetection: UV at 240 nmTemperature: 25 °C

1. Chloramphenicol2. Thiamphenicol

AntibacterialsH250-087

Column: Hypersil GOLD, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: 0.05 M NH4COOH, pH 3

B: ACNIsocratic: 60:40Flow Rate: 1.25 mL/minDetection: UV at 260 nmTemperature: 25 °C

1. Chlorhexidine Digluconate

ChlorhexidineH250-079

Applications


Column: Hypercarb™, 5 µm, 100 x 4.6 mmPart Number: 35005-104630Mobile Phase: A: H2O

B: ACNGradient: 5 to 50% B in 10 minFlow Rate: 1 mL/minDetection: UV at 210 nmTemperature: 40 °C

1. 5,6-Dihydrouracil2. Uracil3. 5-Fluorouracil

Uracil and MetaboliteH350-1087




1. Tablet component2. Tablet component3. Lorazepam

Lorazepam TabletH250-015



B: ACNGradient: Time (min) % B

0 304 305 35

15 70Flow Rate: 1 mL/minDetection: UV at 254 nm

1. Indinavir 4. Amprenavir2. Nelfinavir 5. Ritonavir3. Saquinavir 6. Lopinavir

Protease Inhibitors19100401



B: MeOH + 0.1% Formic acidGradient: 5 to 100% B in 15 minFlow Rate: 1 mL/minDetection: UV at 280 nmTemperature: 40 °C

1. Ascorbic acid2. Phenylephrine3. Acetaminophen (Paracetamol)4. Unknown

Cold RemedyComponents

H250-006



1. t02. Tablet component3. Penicillin V (phenoxymethylpenicillinic acid)

Penicillin V TabletH250-021




1. Timolol 5. Metoprolol2. Atenolol 6. Propranolol3. Nadolol 7. Alprenolol4. Pindolol

Beta BlockersH250-022

Pharma/Biochem




B: ACN + 0.1% Formic acidGradient: 5 to 100% B in 10 minFlow Rate: 6 µL/minDetection: UV at 248 nm

1. Mevastatin (Compactin)2. Lovastatin (Mevinolin)3. Simvastatin

StatinsH250-028




1. Atorvastatin

Atorvastatin H250-029




1. Oxacillin2. Cloxacillin3. Dicloxacillin

Anti-InfectivesH250-030


Part Number: 25005-154630Mobile Phase: A: H2O + 0.05% H3PO4

B: ACN + 0.05% H3PO4

Isocratic: 34:66Flow Rate: 2 mL/minDetection: UV at 214 nm Temperature: 25 °C

1. Ibuprofen

Ibuprofen H250-005


B: TFAC: H2O

Isocratic: 3:0.1:96.9Flow Rate: 1 mL/minDetection: UV at 210 nmSource: C. Lim, IRC, Centre for Mechanism

of Human Toxicity, Leicester, UK

1. Oxalic acid2. Creatine3. Creatinine

Creatine in SerumH350-1054

Column: Hypersil GOLD PFP, 5 µm, 150 x 4.6 mm

Part Number: 25405-154630Mobile Phase: A: 20 mM NH4OAc at pH 8.0


1. Metformin (1,1-Dimethylbiguanide hydrochloride)

MetforminH254-002

Applications




1. Ondansetron

Ondansetron H250-033




1. Clopidogrel hydrogensulphate

ClopidogrelH250-040




1. Ticlopidine hydrochloride2. Clopidogrel hydrogensulphate

Platelet AggregationInhibitors

H250-041


Part Number: 25005-154630Mobile Phase: A: 10 mM NaH2PO4 at pH 2.5

B: MeOH Isocratic: 34:66Flow Rate: 1 mL/minDetection: UV at 254 nmTemperature: 25 °C

1. Diclofenac

DiclofenacH250-010

Fexofenadine Tablet




1. Tablet component2. Fexofenadine3. Tablet component4. Tablet component5. Tablet component

H250-019



B: ACN + 0.1% Formic acidGradient: 5 to 100% B in 15 minFlow Rate: 1 mL/minDetection: UV at 254 nm

1. Guanine2. Acyclovir

AcyclovirH250-004

Pharma/Biochem




B: ACN + 0.1% Formic acidGradient: 50 to 100% B in 10 minFlow Rate: 0.5 mL/minDetection: UV at 254 nmTemperature: 30 °C

1. Itraconazole

ItraconazoleH250-034

Column: Hypersil GOLD, 5 µm, 50 x 2.1 mmPart Number: 25005-052130Mobile Phase: A: 50 mM NH4OAc at pH 9.0

B: ACNGradient: 5 to 100% B in 10 minFlow Rate: 0.2 mL/minDetection: UV at 254 nmTemperature: 30 °C

1. Lansoprazole

Lansoprazole H250-035

Column: Hypersil GOLD, 5 µm, 50 x 2.1 mmPart Number: 25005-052130Mobile Phase: A: 50 mM NH4OAc at pH 9.0


1. Omeprazole2. Lansoprazole

PrazolesH250-036

Minutes0 2 4 6 8 10 12

mVo

lts0

20

40

60

80

Cough and ColdFormulationColumn: Hypersil GOLD™, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: 20 mM NH4COOH at pH 3.0

B: MeOH Gradient: Time (min) % B

0 105 1010 70

Flow Rate: 1.5 mL/minDetection: UV at 270 nmTemperature: 25 °C

1. 4-Amino phenol2. (chlorpheniramine) maleate3. Phenylephrine4. Acetaminophen5. Saccharin6. Impurity from 4-Amino phenol7. 4-Nitro phenol8. Chlorpheniramine

H250-093

1 3

2

4

5

6

7

8


Applications




B: ACN + 0.1% Formic acidIsocratic: 20:80Flow Rate: 1 mL/minDetection: UV at 254 nmTemperature: 30 °C

1. Felodipine

Felodipine H250-038

Column: Hypersil GOLD™, 5 µm, 50 x 2.1 mmPart Number: 25005-052130Mobile Phase: A: 50 mM NH4OAc at pH 9.0

B: ACNIsocratic: 80:20Flow Rate: 0.2 mL/minDetection: + ESI Temperature: 80 °C

1. Enalapril Maleate

Enalapril MaleateH250-037

SulfonamidesColumn: Hypersil GOLD aQ™

5 µm, 150 x 4.6 mmPart Number: 25305-154630Mobile Phase: A: 0.1% Formic acid

B: ACN + 0.1% Formic acidGradient: 10 to 100% B in 15 minFlow: 1.0 mL/minDetection: UV at 270 nmTemperature: 30 °C

1. Sulfaguanidine 4. Sulfamerazine2. Sulfanilamide 5. Sulfamonomethoxine3. Sulfathiazole 6. Sulfaquinoxaline

H253-009


Part Number: 25005-154630Mobile Phase: 0.1% Formic acid


1. Dostinex

Dostinex™ TabletH250-039

Pharma/Biochem


EsomeprazoleColumn: Hypersil GOLD™, 5 µm,

150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: 0.1% NH3 (aq)


1. Esomeprazole

CS002-011




1. Glyburide

GlyburideH250-043


Part Number: 25005-154630Mobile Phase: A: H2O


1. Fluticasone propionate

Fluticasone PropionateH250-044


Part Number: 25005-154630Mobile Phase: A: H20


1. Fluoxymesterone2. Fluorometholone3. Fluticasone propionate

Fluorinated SteroidsH250-046

Applications





1. cis-Diltiazem hydrochloride

Diltiazem H250-042


Part Number: 25005-154630Mobile Phase: A: 0.1% NH3 (aq)

B: MeOH + 0.1% NH3 (aq) Isocratic: 80:20Flow Rate: 1 mL/minDetection: UV at 254 nmTemperature: 40 °C

1. Salmeterol xinafoate

Salmeterol XinafoateH250-047


Part Number: 25003-104630Mobile Phase: A: 50 mM NH4OAc at pH 3.0


1. Chlorhexidine

ChlorhexidineH250-048

XanthinesColumn: Hypersil GOLD aQ™, 5 µm,

150 x 4.6 mmPart Number: 25305-154630Mobile Phase: A: 50 mM NaH2PO4 pH 2.5

B: MeOHGradient: 1-100% B in 10 minFlow Rate: 1 mL/minDetection: UV at 254 nmTemperature: 30 °C

1. Hypoxanthine2. Xanthine3. Theobromine4. Theophylline5. Caffeine

H253-008


Pharma/Biochem





1. Simvastatin

SimvastatinH250-027

Column: Hypercarb™, 5 µm, 100 x 4.6 mmPart Number: 35005-104630Mobile Phase: A: H2O + 0.1% Formic acid

B: ACN + 0.1% Formic acidGradient: 10 to 100% B in 10 minFlow Rate: 0.8 mL/minDetection: UV at 260 nmTemperature: 30 °C

1. Uracil2. 5-Fluorouracil

5-Fluorouracil03100301

Column: Hypersil GOLD CN, 5 µm, 150 x 4.6 mm

Part Number: 25805-154630Mobile Phase: A: 20 mM NH4COOH at pH 3

B: ACNGradient: 0 to 20% B in 15 minFlow Rate: 1 mL/minDetection: UV at 254 nmTemperature: 25 °C

1. Isoniazid2. Pyrazinamide

TuberculostaticsH258-005

1

2

Column: Hypersil GOLD, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: H2O/MeOH (70:30) + 0.1%

Formic acidB: H2O/MeOH (20:80) + 0.1%

Formic acid Gradient: 0-100% B in 15 minFlow Rate: 1.5 mL/minDetection: UV at 220 nmTemperature: 40 °C

1. Caffeine2. Acetylsalicylic Acid3. Bucetin

AnalgesicsH250-081

Column: Hypersil GOLD, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: 0.05 M KH2PO4, pH 3


1. Lidocaine2. Tetracaine3. Benzocaine

AnaestheticsH250-084


B: ACNGradient: 5 – 90% B in 15 minFlow Rate: 1.25 mL/minDetection: UV at 254 nmTemperature: 25 °C

1. Cephalosporin C2. Cephaloridine

Cephalosporin CH250-076

Applications



B: ACNGradient: 10-40% B in 10 minFlow Rate: 1.5 mL/minDetection: UV at 350 nmTemperature: 25 °C

1. Oxytetracycline2. Epi-tetracycline3. Tetracycline4. Methacycline5. Doxycycline

TetracyclinesH250-089

Column: Hypersil GOLD C8, 5 µm, 150 x 4.6 mm

Part Number: 25205-154630Mobile Phase: A: 20 mM NH4OAc pH 4

B: MeOH Gradient: 60-80% B in 10 minFlow Rate: 1.25 mL/minDetection: UV at 230 nmTemperature: 25 °C

1. Carbamazepine2. 10,11-Dihydrocarbamazepine3. Iminostilbene4. Iminodibenzyl

CarbamazepinesH252-003

Column: Hypersil GOLD, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: 0.01% TFA

B: 0.01% TFA in ACNGradient: 15-70% B in 20 minFlow Rate: 1 mL/minDetection: UV at 230 nmTemperature: 25 °C

1. Angiotensin III2. Angiotensin II3. Angiotensin I

AngiotensinsH250-063


Part Number: 25005-154630Mobile Phase: A: 0.05 M NH4COOH, pH 3.5

B: ACNGradient: 10-50% B in 10 minFlow Rate: 1.5 mL/minDetection: UV at 254 nmTemperature: 25 °C

1. Uracil2. Procainamide3. Acetyl-Procainamide4. Caffeine5. Propionyl Procainamide

ProcainamidesH250-064



1. Furazolidone2. Oxolinic Acid3. Nalidixic Acid

AntibacterialsH250-068

Column: Hypersil GOLD, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: 0.05 M NH4COOH, pH 3

B: ACNGradient: Time (min) %B

0 1015 2520 10


1. Pseudoephedrine HCl2. Chlorpheniramine Maleate

AntihistaminesH250-069

Pharma/Biochem


Bile AcidsColumn: Hypersil™ ODS, 3 µm, 100 x 1.0 mmPart Number: 30103-101030Mobile Phase: A: 0.1M NH4OAc buffer at pH 4.8

with 2% Glycerol matrixB: MeOH with 2% Glycerol matrix

Gradient: 55 to 75% B in 45 minFlow Rate: 60 µL/minDetection: Continuous Flow FAB MSSource: Evans, J.E., Biolog. Mass

Spectrom, 22, 331 (1993)

Bile acids – extract of urine from patient with NALD

5049

Penicillin V TabletColumn: Hypersil GOLD™ CN, 5 µm,

150 x 4.6 mmPart Number: 25805-154630Mobile Phase: A: 10 mM KH2PO4 at pH 3


1. Penicillin V

H258-007


Applications


Ribonucleotides

Column: Hypercarb™, 5 µm, 30 x 3.0 mmPart Number: 35005-033030Mobile Phase: A: 50 mM NH4OAc at pH 6.0

B: ACNGradient: 5 to 70% B in 7 minFlow Rate: 0.5 mL/minDetection: + ESI

H350-1019

1. Cytidine 5'- monophosphate2. Cytidine 3'- monophosphate3. Cytidine 3', 5'- cyclic monophosphate

1. Guanosine 5'- monophosphate2. Guanosine 3'- monophosphate3. Guanosine 2',3'- cyclic monophosphate4. Guanosine 2'- monophosphate5. Guanosine 3', 5'- cyclic monophosphate

1. Adenosine 5'- monophosphate 2. Adenosine 3'- monophosphate 3. Adenosine 3', 5'- cyclic monophosphate

a b c

a

b c

PTH Amino AcidsColumn: Hypersil GOLD™, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: 0.1% TFA + 0.015%

Triethylamine in H2OB: 0.1% TFA + 0.015%

Triethylamine in ACNGradient: Time (min) % B

0 172 207 35

20 35Flow Rate: 1 mL/minDetection: UV at 269 nmTemperature: 25 °C

1. Serine 6. Tyrosine2. Asparagine 7. Methionine3. Aspartic acid 8. Tryptophan4. Glutamic acid 9. Phenylanaline5. Alanine 10. Leucine

H250-096

Pharma/Biochem


Oligosaccharidesfrom a GlycoproteinColumn: Hypercarb™, 5 µm, 100 x 1.0 mmPart Number: 35005-101030Mobile Phase: A: 5 mM NH4OAc at pH 9.6 +

2% ACNB: 5 mM NH4OAc at pH 9.6 +

80% ACNGradient: 5 to 40% B in 80 minFlow Rate: 50 µL/minDetection: + ESISource: Nana Kawasaki, National

Institute of Health Science, Tokyo, Japan

Reduced N-linked oligosaccharides from:(A) RNase B(B) Desialylated rhEPO(C) Fetuin(D) Sialylated rhEPO

07100302

Underivatized Amino AcidsColumn: Hypercarb, 5 µm, 100 x 2.1 mmPart Number: 35005-102130Mobile Phase: A: 20 mM Nonafluoropentanoic acid

(NFPA) (aq)B: ACN

Gradient: Time (min) % B0 0

10 1520 2630 50

Flow Rate: 0.2 mL/minDetection: ELSD (55 °C, 2.2 bar)Temperature: 10 °CSource: Prof. Dreux, Univ. D’Orleans, France

1. Glycine 9. Glutamine 17. Arginine2. Serine 10. Glutamic acid 18. Phenylalanine3. Alanine 11. Valine 19. Tyrosine4. Threonine 12. Lysine 20. Impurity5. Cysteine 13. Leucine 21. Impurity6. Asparagine 14. Methionine 22. Tryptophan7. Aspartic acid 15. Isoleucine8. Proline 16. Histidine

H350-1049

Applications


Column: BioBasic™ AX, 5 µm, 150 x 4.6 mmPart Number: 73105-154630Mobile Phase: A: 5 mM KH2PO4 at pH 3.2

B: 750 mM KH2PO4 at pH 3.2Gradient: 0 to 100% B in 30 minFlow Rate: 1 mL/minDetection: UV at 254 nmTemperature: 25 °C

1. Cytidine-3-monophosphate 7. Uridine-5-diphosphate2. Uridine-5-monophosphate 8. Guanosine-5-diphosphate3. Adenosine-5-monophosphate 9. Cytidine-5-triphosphate4. Guanosine-5-monophosphate 10. Adensosine-5-triphosphate5. Cytidine-5-diphosphate 11. Uridine-5-triphosphate6. Adenosine-5-diphosphate 12. Guanosine-5-triphosphate

NucleotidesK731-001

Column: BioBasic AX, 5 µm, 50 x 4.6 mmPart Number: 73105-054630Mobile Phase: A: 5 mM KH2PO4 at pH 7.2

B: 150 mM KH2PO4 at pH 7.2Gradient: 75 to 100% B in 15 minFlow Rate: 0.4 mL/minDetection: UV at 265 nm

1. 10-mer 5. 15-mer2. 12-mer 6. 16-mer3. 13-mer 7. 17-mer4. 14-mer 8. 18-mer

OligonucleotidesK731-014

Column: BioBasic SCX, 5 µm, 150 x 4.6 mmPart Number: 73205-154630Mobile Phase: A: 20 mM Tris buffer at pH 6

B: A + 1.0 M sodium acetate at pH 6

Gradient: 0 to 100% B in 60 minFlow Rate: 1 mL/minDetection: UV at 280 nm

1. Trypsinogen 4. Cytochrome C2. Ribonuclease A 5. Lysozyme3. Chymptrypsinogen A

ProteinsK732-002

Column: BioBasic SEC 1000, 5 µm, 300 x 7.8 mm

Part Number: 73605-307746Mobile Phase: 0.1 M KH2PO4 at pH 7Flow Rate: 1 mL/minDetection: UV at 280 nm

1. Thyroglobulin2. Ovalbumin3. PABA

Proteins and Peptides by SEC

K736-003



1. Thyroglobulin2. Ovalbumin3. Myoglobulin4. Aprotinin5. Neurotensin6. PABA


K734-001

0 2 4 6 8 10 12 MIN

12

3

0 2 4 6 8 10 12 14 MIN

1

2 3

45

6

0 5 10 15 20 25 30 35 40

1

2

3

4

5

Column: BioBasic SCX, 5 µm, 150 x 4.6 mmPart Number: 73205-154630Mobile Phase: A: 100 mM ammonium acetate,

pH 4.0B: ACN

Isocratic: 98:2Flow Rate: 1.0 mL/minDetection: MS +ESI Temperature: 25 °C

1. Betaine

Betaine – A Hepatosupressant

H732-001


Pharma/Biochem


Substituted PeptidesColumn: BioBasic™ SCX, 5 µm, 50 x 4.6 mmPart Number: 73205-054630Mobile Phase: A: 10 mM KH2PO4 in 25% ACN at

pH 4.8 (phosphoric acid)B: A + 0.5 M NaCl

Gradient: 0 to 50% B in 20 minFlow Rate: 1 mL/minDetection: UV at 210 nm

1. Ac-G-G-G-L-G-G-A-G-G-L-K-amide2. Ac-K-Y-G-L-G-G-A-G-G-L-K-amide3. Ac-G-G-A-L-K-A-L-K-G-L-K-amide4. Ac-K-Y-A-L-K-A-L-K-G-L-K-amide

K732-005

0 2 4 6 8 10 12 14 16 18 MIN

3

2

1

4

CeramidesColumn: Hypercarb™, 5 µm, 100 x 2.1 mmPart Number: 35005-102130Mobile Phase: A: MeOH

B: CHCl3Gradient: 45 to 80% B in 15 minFlow Rate: 0.4 mL/minDetection: ELSD Temperature: 50 °CSource: K. Gaudin, Laboratoire de Chimie

Analytique, Université Paris Sud, France

H350-1080

Ceramides:1. d18:1c16:02. d18:0c16:03. d18:1c18:04. d18:0c18:05. d18:1c22:1

6. d18:1c20:07. d18:1c23:18. d18:1c24:19. d18:1c22:010. d18:1c25:1

11. d18:1c23:012. d18:1c26:113. d18:1c24:014. d18:1c25:015. d18:1c26:0

Tryptic Digest of CaseinColumn: Hypercarb, 5 µm, 50 x 2.1 mmPart Number: 35005-052130Mobile Phase: A: H2O + 0.05% TFA

B: ACN:H2O (9:1) + 0.035% TFAGradient: Time (min) % B

0 03 0

23 90Flow Rate: 0.7 mL/minDetection: UV at 195 nm; +ESITemperature: 25 °C

Casein Tryptic Digest

H350-003

www.thermo.com /columns

Applications

253



1. Adrenaline2. Dopamine3. L-Dopa

CatecholaminesH350-1005

Column: BioBasic AX, 5 µm, 150 x 4.6 mmPart Number: 73105-154630Mobile Phase: A: 20 mM Tris buffer at pH 6

B: A + 1M NaOAc at pH 6Gradient: 0 to 100% B in 40 minFlow Rate: 1 mL/minDetection: UV at 280 nm

1. β-lactoglobulin B2. β-lactoglobulin A

ProteinsK731-005

Column: BioBasic™ SEC 60, 5 µm, 300 x 7.8 mm


1. Thyroglobulin2. Neurotensin3. Angiotensin II4. PABA


K733-001

Column: Hypercarb, 3 µm, 100 x 0.32 mmPart Number: 35003-100330Mobile Phase: A: 0.5% Formic acid


1. Norepinephrine2. Epinephrine3. Dopamine4. L-Dopa5. Serotonin6. DOPAC

19070403

Catecholamines


Part Number: 73505-153030Mobile Phase: A: 50 mM KH2PO4 at pH 3.5

B: ACNIsocratic: 90:10Flow Rate: 0.5 mL/minDetection: UV at 220 nm

1. Dextromethorphan 3. Nortriptyline2. Propranolol

Direct Serum Injectionfor Drug Analysis

K733-004

0 2 4 6 8 Min

1

2

3

200 ng each in 10 mL Bovine Serum

Column: BioBasic AX, 5 µm, 150 x 4.6 mmPart Number: 73105-154630Mobile Phase: A: 10 mM NH4OAc


1. Cephaloridine 4. Cephalosporin C2. Amoxicillin 5. N-acetylpenicillamine3. Ampicillin 6. Penicillin G

AntibioticsK731-004

Pharma/Biochem


Column: Hypercarb, 5 µm, 50 x 2.1 mmPart Number: 35005-052130Mobile Phase: A: 20 mM NH4OAc at pH 6

B: ACNGradient: 5 to 100% B in 5 minFlow Rate: 0.3 mL/minDetection: + ESITemperature: 35 °C

1. Thr-Ser-Lys2. Arg-Gly-Glu-Ser3. Asp-Ser-Asp-Pro-Arg

Hydrophilic PeptidesH350-1014

Column: BioBasic™ C4, 5 µm, 150 x 4.6 mmPart Number: 72305-154630Mobile Phase: A: 0.1% TFA

B: ACN + 0.1% TFAGradient: 5 to 50% B in 40 minFlow Rate: 1 mL/minDetection: UV at 220 nm

Tryptic digest of BSA

Tryptic Digest of BSAK723-001

Column: Hypercarb™, 5 µm, 100 x 4.6 mmPart Number: 35005-104630Mobile Phase: A: H2O + 0.1% TFA

B: H2O:ACN (20:80) + 0.085% TFAGradient: 0 to 100% B in 30 minFlow Rate: 1 mL/minDetection: UV at 254 nmTemperature: 37 °CSource: Günter Lochnit, Institute de

Biochimie, Université de Justus-Liebig, Giessen

1. CDP-choline2. GDP-choline3. UDP-choline4. ADP-choline

Choline DerivatizedNucleotides

H350-1079

Column: Hypercarb, 5 µm, 100 x 4.6 mmPart Number: 35005-104630Mobile Phase: A: H2O

B: ACNGradient: 10 to 50% B in 50 minFlow Rate: 1 mL/minDetection: UV at 210 nmTemperature: 40 °CSource: J. Fan and A. Kondo, Anal.

Biochem. 219, 224 (1994).Reproduced with permission

1. R-I (Man6GlcNAc2Asn)2. R-II (Man5GlcNAc2Asn)3. R-III (Man6GlcNAc2AsnLeu)4. R-IV (Man5GlcNAc2AsnLeu)

RNB-Glycopeptides07100301

Column: Hypercarb, 5 µm, 100 x 4.6 mmPart Number: 35005-104646Mobile Phase: H2OFlow Rate: 2 mL/minDetection: UV at 254 nmTemperature: 150 to 200 °C at 15 °C/min;

hold at 200 °C

1. Cytosine 4. Hypoxanthine2. Uracil 5. Guanine3. Thymine 6. Xanthine

Purines and Pyrimidines(UHT-LC)

H350-1102

Column: Hypersil GOLD™, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: 35.1 g Sodium Perchlorate, 1.4 g

KH2PO4, 40 mL MeOH, 7 mL 1 MKOH – made up to 1 liter, pH 7.2


1. Folic Acid

Minutes0 1 2 3 4 5 6 7 8

Folic Acid USP MethodH250-077 1

Applications



B: ACN Gradient: 15 to 100% B in 2 minFlow Rate: 0.4 mL/minDetection: - ESI Temperature: 25 °C

1. Cytidine2. Uridine3. Guanosine4. Adenosine

NucleosidesH350-1001


B: ACN + 0.1% Formic acidGradient: 10 to 30% B in 10 minFlow Rate: 6 µL/minDetection: UV at 254 nmTemperature: 25 °C

1. dCMP2. dUMP3. dAMP4. dGMP

2'-Deoxynucleoside 5'-Monophosphates

H350-1047

Column: Hypercarb, 5 µm, 100 x 0.32 mmPart Number: 35005-100365Mobile Phase: A: 20 mM NH4OAc pH 5.5

B: ACNGradient: 10 to 30% B in 15 minFlow Rate: 6 µL/minDetection: UV at 254 nm

1. 3',5'-cCMP2. 3',5'-cUMP3. 3',5'-cGMP4. 3',5'-cAMP


Part Number: 73505-307846Mobile Phase: 0.1 M KH2PO4 pH 7Flow Rate: 1.0 mL/minDetection: UV at 280 nm

1. Thyroglobulin2. β-Amylase3. BSA4. Ovalbumin5. Myoglobulin6. Aprotinin7. Angiotensin II8. PABA

ProteinsK735-002comp

Column: Hypercarb, 5 µm, 100 x 0.32mmPart Number: 35005-100365Mobile Phase: A: H2O + 0.1% Formic acid


1. Cytosine2. Uracil3. Guanine4. Adenine5. Xanthine6. Thymine

Purines and PyrimidinesH350-1041

Nucleoside 3', 5'-CyclicMonophosphates

H350-1040

Column: Hypercarb, 3 µm, 100 x 2.1 mmPart Number: 35003-102130Mobile Phase: A: 10 mM NH4COOH at pH 3.5

B: ACNGradient: 10 to 50% B in 10 minFlow Rate: 150 µL/minDetection: + ESITemperature: 40 °C

1. L-arginine2. Methyl-L-arginine3. Asymmetrical dimethyl arginine

01030403

Arginine andMethylated Arginines

Pharma/Biochem


Bacterial Acid Methyl EstersColumn: TR-FAME, 30 m x 0.25 mm

x 0.25 µmPart Number: 260M142PTemperature: 100 °C 1 min, 5 °C/min to 220 °CDetector Type: FIDInjection Mode: Split

260M010

1. C11:02. C12:03. C13:04. C10:0 2-OH5. C14:06. C15:0-i7. C15:0-a8. C15:09. C12:0 2-OH10. C16:0-i11. C16:012. C15.1n7-cis13. C12:0 3-OH14. C17:0-a

15. C17:016. C9,10-methylene 16:017. C14:0-2-OH18. C18:019. C18:1n9-trans20. C18.1n9-cis21. C18.1n7-cis22. C18.2n6-cis23. C19:024. C16:0 2-OH25. C9,10-methylene 18:026. C20:027. C18:0 2-OH

Residual Solvents inPharmaceuticalsColumn: TR-V1 30 m x 0.32 mm x 1.8 µmPart Number: 260V339PTemperature: 35 °C, hold 4 min, 30 °C/min to

90 °C, hold 1 min, 30 °C/min to110 °C, no hold, 45 °C/min to170, hold 1 min. (Inlet 200 °C)

Detector Type DSQ MSCarrier Gas: HeFlow Rate 6 mL/minInjection Type: HeadspaceInjection Mode: Split, 5:1

1. Methanol2. Methylene Chloride3. Acetonitrile4. 1,2-dichloroethene5. Hexane6. 1,1-dichloroethene7. Chloroform8. Nitromethane9. 1,1,1-trichloroethane10. Cyclohexane11. carbon tetrachloride12. Benzene13. 1,2-dimethoxy ethane14. 1,2-dichloroethane

15. trichloroethene16. methyl cyclohexane17. 1,4-dioxane18. 2-ethoxy ethanol19. Toluene20. Pyridine21. Hexanone22. Chlorobenzene23. Ethylbenzene24. m-Xylene25. p-Xylene26. dimethyl acetamide27. 1-methyl 2-pyrrolidinone28. tetra-hydro-naphthalene

Applications


Partially MethylatedGlucoseColumn: TR-FAME, 25 m x 0.22 mm x 0.25 µmPart Number: 260M135PTemperature: 185 °C 1 min, 3 °C/min to 260 °C,

hold 10 minDetector Type: MSDetection: 70 eV, 100-350 m/zCarrrier Gas: He, 50 kPaInjection 1 µLVolume:Injection SplitMode:

260M011

1. 2,3,4-O-methyl rhamnitol2. 2,3,5-O- methyl arabinitol (f)3. 2,3,4-O-methyl arabinitol (p)4. 3,5-O-methyl arabinitol5. 2,3,4,6-O-methyl glucitol6. 2,5-O-methyl arabinitol7. 2,3,4,6-O-methyl galactitol8. 2,3-O-methyl arabinitol9. 2,4,6-O-methyl galactitol10. 2-O-methyl arabinitol

11. 2,3,6-O-methyl glucitol12. 2,3,4-O-methyl galactitol13. arabinitol hexa-acetate14. xylitol hexa-acetate15. 2,3,4,6-O-methyl galactitol16. 2-O-methyl galactitol17. 4-O-methyl galactitol18. Galactitol hexa-acetate19. Glucitol hexa-acetate20. Myo-inositol hexa-acetate


SPE-LC/ESI/MS Method for the Analysis of Polar Micro Pollutants inEnvironmental WatersAn SPE-LC/ESI/MS method for the analysis of polar degradation products of atrazine allowstheir determination in environmental waters at the 0.1 μg/L level.

Increasingly, environmental protection legislation designates maximumlevels permitted for micro-pollutants in water below the µg/L level.These detection levels require sample preparation and pre-concentrationbecause they are too dilute. In solid phase extraction (SPE), the analytes are extracted provided they are retained by the sorbent andnot eluted too rapidly by the water in the sample. However, traceanalysis of very polar pollutants is still a challenge, since traditionalC18-silica and PS-DVB materials do not adequately retain these compounds.1 Porous graphitic carbon (PGC, Hypercarb) retains highlypolar and water-soluble compounds and is useful for the trace-leveldetermination of polar water pollutants.

This application presents a SPE procedure and LC/ESI/MS methodusing Hypercarb for the analysis of polar degradation products ofatrazine (ammeline - ANE, ammelide - ADE, atrazin-desethyl-desiso-propyl - DEIA, atrazin-desethyl - DEA, atrazin-desisopropyl - DIA, Cyanuricacid - Cya) that allow their detection in water at the 0.1 µg/L level.

Experimental ConditionsSPE

Compounds: ANE, ADE, DEIA, DEA, DIA, Cyanuric acidPhase: HyperSep™ Hypercarb™

Part Number: 60106-402Volume: 6 mLBed Weight: 500 mgConditioning: 10 mL MeOH followed by 10 mL H2O, vacuum at 3 mm HgApplication: 500 mL, vacuum at 10 mm HgElution: 6 mL (MeOH/THF, 1:1) + 0.1% TFA (stand for 1 min,

vacuum at 3 mm Hg), 6 mL (MeOH/THF, 1:1) + 0.1% TFA(vacuum at 3 mm Hg).

The sample was dried under nitrogen and re-dissolved in 1 mL of H2O.

LC/ESI/MS

Column: Hypercarb 5 µm, 100 x 2.1 mmPart Number: 35005-102130Instruments: Surveyor™ HPLC and LCQ™ Deca MSMobile Phase: A: H2O + 0.1% Formic acid

B: ACN + 0.1% Formic acidGradient: 10 to 100% B in 10 min Flow Rate: 0.2 mL/minInjection Volume: 10 µLDetection: + ESI (SIM MS ([M + H]+) for ANE, ADE, DEIA, DEA, DIA;

- ESI ([M - H]-) for cyanuric acidTemperature: 68 °C

Results and DiscussionA typical trace for the separation in LC/ESI/MS is shown in Figure 1.Average recoveries for a pre-concentrated, 500 mL of water spikedwith 0.1 µg/L each of the six polar degradation compounds rangedbetween 75 and 100%. These results demonstrate that the use ofPGC in SPE to extract very polar pollutants from water will allow theloading of high volumes of water when target analyte pre-concentra-tion is required to detect trace pollutants. Also PGC as a stationaryphase for the LC separation retains very polar molecules and allows the use of weakly buffered mobile phases ideal for sensitiveMS detection.

References1. Pichon, L. Chen, S. Guenu, and M.C. Hennion, J. Chromatogr. A, 711, pp 257–267 (1995)

0

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Figure 1: LC/ESI/MS trace for standard solution containing the six pollutants.

H350-1131

Analytes: 1. ANE; 2. ADE; 3. Cyanuric acid; 4. DEIA; 5. DEA; 6. DIA.

Environmental


EPA Method 610: Increasing Analysis ThroughputVarying GC column dimensions and running conditions can significantly reduce run timesleading to increased throughput.

The pressure of heavy workload and the continuing need to improveproductivity in a modern environmental laboratory requires a highthroughput of samples. With advances in sample preparation methods,GC analysis time is becoming the rate-determining step for manyanalyses.

This application note demonstrates the combination of severalmethod approaches for speeding up environmental analyses usingtwo TRACE™ TR-5MS (5% phenyl polysiphenylene-siloxane coated)columns. The key outcome is the reduction in analysis time whilemaintaining resolution, elution order and sensitivity, using readilyavailable techniques such as alteration of column length, oven temperature ramp, column ID and film thickness. The sample used for the comparison is the 16 component standard mixture used in EPA 610 (polynuclear aromatic hydrocarbons).

Experimental ConditionsOriginal GC Method (1a)

Instrument: TRACE GC Ultra™

Column: TRACE TR-5MS, 30 m x 0.25 mm x 0.25 µmPart Number: 260F142PInitial Temp.: 100 °C Rate 1: 5 °C/min to 300 °C Carrier Gas: He Flow Rate: 1.5 mL/minInjection Volume: 1 µL Split Ratio: 50:1Detection: FID

Fast GC Method (1b)

Instrument: TRACE GC UltraColumn: TRACE TR-5MS, 10 m x 0.1 mm x 0.1 µmPart Number: 260F020PInitial Temp.: 150 °C Rate 1: 45 °C/min to 330 °C Carrier Gas: He Flow Rate: constant pressure 780 kPaInjection Volume: 1 µLSplit Ratio: 50:1Detection: FID

Results and DiscussionFigure 1 illustrates the reduction in analysis time from 45 to 5 minutesby decreasing the column length, ID and film thickness and simultane-ously using a faster temperature program and running at constantpressure, which increases the linear velocity at the beginning of therun where the peaks are well separated.

Figure 1: Reduction of analysis time for 16 PAHs from 45 minutes with conventional method to 5 minutes.

(a)

(b)

1. Naphthalene 2. Acenaphthylene 3. Acenaphthene 4. Fluorene 5. Phenanthrene 6. Anthracene 7. Fluoroanthene 8. Pyrene9. Benzo (a) anthracene 10. Chrysene 11. Benzo (b) fluoroanthene12. Benzo (k) fluoroanthene13. Benzo (a) pyrene 14. Dibenzo (a,h) anthracene 15. Indeno (1,2,3-cd) pyrene 16. Benzo (ghi) perylene

260F103

260F102

Applications


Rapid Analysis of Priority Phenolic Pollutants with Hypersil GOLD 1.9 μm and U-HPLCTransferring a method for the analysis of priority phenolic pollutants using Hypersil GOLDcolumns to U-HPLC significantly increases analysis speed and sensitivity

Phenolic compounds are of environmental importance due to their relatively high toxicity at low levels and their presence in environmentalwaters and organic matter, following degradation of a range of industrial products such as pesticides and herbicides.

Reverse-phase liquid chromatography (RP-LC) has been shown toeffectively separate and detect a range of phenolic compounds at lowppb levels, following various extraction methods. Such methods providea realistic alternative to traditional analytical approaches using gaschromatography (GC), which tend to be hindered by lengthy samplepreparation/analysis times and difficulty in derivitization of certainphenols. We now demonstrate the effect of using Hypersil GOLD and1.9 µm particles on the separation and analysis speed of a number ofpriority phenols cited within the US Environmental Protection Agency(EPA) and European Union (EU) lists of priority pollutants.1, 2

Experimental ConditionsStandard HPLC Conditions

Instrument: Surveyor™ LCColumn: Hypersil GOLD™ 5 µm, 150 x 2.1 mmPart Number: 25005-152130Mobile Phase: A: H2O + 0.1% Acetic acid

B: MeOH + 0.1% Acetic acidGradient: 5% B (Hold for 1.5 mins) to 95% B on 19.5 mins

(Hold for 1.5 mins)Flow Rate: 0.6 mL/minInjection Volume: 10 µLDetection: UV diode array (270-320 nm)Temperature: 60 °C

U-HPLC Conditions

Instrument: Accela™ High Speed LCColumn: Hypersil GOLD 1.9 µm, 100 x 2.1 mmPart Number: 25002-102130Mobile Phase: A: H2O + 0.1% acetic acid

B: MeOH + 0.1% acetic acidGradient: 5% B (Hold for 0.6 mins) to 95%B on 7.8 mins

(Hold for 0.6 mins)Flow Rate: 1.0 mL/minInjection Volume: 1 µLDetection: UV diode array (270-320 nm)Temperature: 60 °C

Results and DiscussionA number of priority phenols can be successfully separated usingHypersil GOLD columns. Method transfer from 5 µm to 1.9 µm particlesand shorter column lengths allows significantly faster analysis times(a reduction of approximately three times in this example), whilemaintaining excellent resolution and reducing peak widths, resultingin increased peak heights and improved sensitivity.

References1. N. Jones et al Poster presented at HPLC 2007, Ghent, Belgium (Reference:

PO20390_E06/07).2. US Environmental Protection Agency Method 625, 1984.

Figure 1: Separation of eleven priority phenolic pollutants. Analysis time isreduced from 17 to 7 minutes.

Analytes: 1. Phenol; 2. 4-Nitrophenol; 3. 2,4-Dinitrophenol; 4. 2-Nitrophenol; 5. 4-Methylphenol; 6. 4-Chlorophenol; 7. 2-Chlorophenol; 8. 2,4-Dimethylphenol; 9. 2,4-Dichlorophenol; 10. 2,4,6-Trimethylphenol; 11. Pentachlorophenol. Prepared in Water: Methanol (95:5) at approx. 5 ppm.

Standard HPLCHypersil GOLD 5 µm particles

U-HPLCHypersil GOLD 1.9 µm particles

H250-124

H250-126

Environmental


Applications


Environmental

Cyanuric Acid inDrinking WaterCompounds: Cyanuric AcidPart Number: 60106-402Phase: HyperSep™ Hypercarb™

Volume: 6 mLBed Weight: 500 mgSample Adjust water sample to pH 3Pretreatment:Conditioning: Wash column with 10 mL methanol

Condition column with 10 mL LC-grade water

Application: Force/aspirate 250-500 mL of water sample into column at rateof 5 mL/min

Washing: Dry column under vacuumElution: 20 mL methanol – evaporate to

dryness at 50 °C under nitrogenSource: Marie Claire Hennion, ESPCI, Paris

OrganochlorineInsecticides from WaterCompounds: Aldrin, p,p'-DDE, o,p'-DDE, o,p'-DDT,

p,p'-DDT, dieldrin, endosulfan I,endosulfan II, endrin, heptachlor,heptachlor epoxide, lindane, p,p'-methoxychlor

Part Number: 60108-305Phase: HyperSep C18Volume: 6 mLBed Weight: 500 mgSample Filter sample if requiredPretreatment:Conditioning: 12 mL ethyl acetate followed by

6 mL methanol and 6 mL distilledwater

Application: Force or aspirate sample slowly through column.

Washing: 6 mL distilled water – dry column under vacuum for 15 min

Elution: 2 x 500 µL ethyl acetateConcentrate eluate to 250 µL instream of nitrogen at 40 °C.

Trace Metal Elementsfrom WaterCompounds: Bi, Cd, Co, Cu, Fe, Hg, Mn, Mo,

Ni, Pb, TiPart Number: 60108-388Phase: HyperSep PhenylVolume: 3 mLBed Weight: 500 mgSample Adjust 500 mL water to pH 8-9 Add Pretreatment: 1 mL 0.1% aqueous sodium diethyl

dithiocarbamate solutionConditioning: 3 mL methanol followed by

3 mL waterApplication: Force or aspirate sample through

column at rate of 3-4 mL/minWashing: 2 mL distilled water. Dry column

under vacuum for 3-4 min.Elution: 6 mL Methanol

Explosives from WaterCompounds: 1,3-dinitrobenzene, 2,6-dinitro-

toluene, 2,4-dinitrotoluene,nitrobenzene, RDX (hexahydro-1,3,5-trinitro-s-triazine), tetryl (N-methyl-N,2,4,6-tetranitroaniline), 1,3,5-trinitrobenzene, 2,4,6-trinitrotoluene

Part Number: 60108-305Phase: HyperSep C18Volume: 6 mLBed Weight: 500 mgSample Adjust 500 mL water sample Pretreatment: to pH 6 Dissolve 150 g NaCl in

the sample and filterConditioning: 12 mL methanol followed by

12 mL waterApplication: Force or aspirate sample slowly

through columnWashing: 1 mL distilled water. Dry column

under vacuum for 5 minElution: 2 x 1 mL volumes methanol

Extraction of Tear GasCompounds: Chloroacetophenone (cs),

o-chlorobenzylidenemalonitrile (cn),trans-8-methyl-n-vanillyl-6-none-namide (oc)

Part Number: 60108-742Phase: HyperSep Verify™-CXVolume: 10 mLBed Weight: 200 mgSample Clothing: Cut out portion of sprayedPretreatment: area and a ‘negative’ control

sample. Extract each into hexaneCanisters: Spray onto a Kimwipe™

and extract sprayed area and anegative control sample into hexane.

Conditioning: 3 mL CH3OH followed by 3 mLdeionized water and 1 mL 100 mMphosphate buffer (pH 6)

Application: Load at 1 mL/minWashing: 3 mL deionized water and 3 mL

hexane. Dry column for 5 min at >10inches Hg

Elution: 1 mL CH3OHEvaporate to dryness at < 40 °C

Pesticides and PAHsfrom WaterCompounds: Pesticides, PAHsPart Number: 60108-302Phase: HyperSep C18Volume: 1 mLBed Weight: 100 mgConditioning: 1 mL methanol followed by 1 mL

distilled waterApplication: Force or aspirate 50-100 mL water

through columnWashing: Dry column under vacuumElution: Pour 500 µL ethyl acetate into

column. Allow to percolate without vacuum. Collect eluate for subsequent analysis


Environmental


Column: Hypersil GOLD™, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: H2O

B: ACN Gradient: 25-70% B in 20 minFlow Rate: 1.5 mL/minDetection: UV at 220 nmTemperature: 25 °C

1. Desethyl atrazine 5. Diuron2. Estriol 6. Bisphenol A3. Simazine 7. Estrone4. Atrazine

Endocrine DisruptersH250-090

Column: BioBasic™ SCX, 5 µm, 150 x 4.6 mmPart Number: 73205-154630Mobile Phase: 300 mM KClFlow Rate: 0.8 mL/minDetection: UV at 290 nmTemperature: 30 °C

1. Diquat2. Paraquat

Quaternary AmineHerbicides

H732-002


B: ACN:IPA (1:3)Gradient: 35 to 95% B in 10 minFlow Rate: 1 mL/minDetection: UV at 240 nmTemperature: 60 °C

1. Prometon 4. Simazine2. Propazine 5. Ametryn3. Prometryn 6. Simetryn

TriazinesH350-1029



B: ACNGradient: Time (min) % B

0 2015 2325 75


1. Simazine 5. Diuron2. Monuron 6. Propazine3. Chlorotoluron 7. Linuron4. Atrazine

Triazine and UronHerbicides

H252-0101

2



B: ACNGradient: 60 to 90% B in 10 min; hold 10 minFlow Rate: 1 mL/minDetection: UV at 254 nmTemperature: 25 °C

PhthalatesH252-006

1. Dimethyl phthalate2. Diethyl phthalate3. Dipropyl phthalate

4. Diisopropyl phthalate5. Di-n-butyl phthalate6. Di-n-octyl phthalate

Applications



B: 50 mM Na2HPO4 at pH 7.0Isocratic: 30:70Flow Rate: 1 mL/minDetection: UV at 210 nmSource: Marie Claire Hennion, ESPCI,

Paris, France

1. Cyanuric Acid Samples:a) Extracted blankb) Water spiked with cyanuric acid

Cyanuric Acid inDrinking Water

7031

QuaternaryAmmonium Salts

28070401

Linear OligoglycerolsColumn: Hypercarb™, 5 µm, 100 x 4.6 mmPart Number: 35005-104630Mobile Phase: A: H2O

B: ACNGradient: 0 to 30% B in 30 minFlow Rate: 1 mL/minDetection: ELSD Source: Mr. Lafosse, ICOA Orléans,

and Mme. Debaig, ENSCR Rennes, France

1. NaCI2. Diglycerols3. Triglycerols4. Tetraglycerols5. Pentaglycerols

04060301

Column: Hypercarb, 5 µm, 50 x 4.0 mmPart Number: 35005-054030Mobile Phase: A: H2O + 0.05% TFA

B: ACN + 0.05% TFAGradient: 5 to 35% B in 10 minFlow Rate: 0.8 mL/minDetection: UV at 295 nm to 3 min, 245 nm

from 3 to 10 minTemperature: 25 °C

1. Diquat

2. Paraquat

Column: Hypersil GOLD™, 3 µm, 150 x 2.1 mmPart Number: 25003-152130Mobile Phase: A: 25 mM NH4OAc at pH 5

B: ACNGradient: 20 to 100 % B in 10 minFlow Rate: 0.2 mL/minDetection: UV at 254 nmTemperature: 40 °C1. 2,4-Diaminotoluene2. 4,4'-Oxydianiline3. o-Toluidine4. 2-Methoxy-5-methylaniline5. 2,4,5-Trimethylaniline6. 4,4'-Methylene-bis(2-chloroaniline)7. Unknown

Banned Aromatic AminesH250-026

1

Environmental



B: ACN + 0.1% Formic acid Gradient: 5 to 100% B in 10 minFlow Rate: 0.3 mL/minDetection: + ESI

1. Aminomethylphosphonic acid (AMPA)

2. Glyphosate

Glyphosate and AMPAH350-1050

1. Solvent front2. Bentazone3. Dicamba

4. MCPP5. MCPA6. 2,4-D

7. MCPB8. Benazolin

1. Naphthalene2. Fluorene

3. Phenanthrene4. Anthracene

5. Pyrene6. Chrysene

Column: Hypersil GOLD™, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: MeOH

B: H2OIsocratic: 75:25Flow Rate: 1 mL/minDetection: UV at 269 nmTemperature: 25 °C

PAHsH250-058

Column: Hypercarb, 5 µm, 50 x 4.6 mmPart Number: 35005-054646Mobile Phase: A: H2O + 0.1% TFA

B: ACN + 0.1% TFAIsocratic: 20:80Flow Rate: 2 mL/minDetection: UV at 205 nmTemperature: 70 to 160 °C at 40 °C/min

Phenoxy Acids (UHT-LC)H350-1115

Column: Hypercarb, 3 µm, 100 x 0.32 mmPart Number: 35003-100365Mobile Phase: A: 0.1% Formic acid


Sample: p-Nonylphenol (some of the possible isomer structuresrepresented below)

Nonylphenol Isomers12020401

Column: Hypercarb, 7 µm, 100 x 4.6 mmPart Number: 35007-104630Mobile Phase: A: ACN

B: 8 mM H3PO4

Isocratic: 5:95Flow Rate: 1 mL/minDetection: EC (0.35 V)Source: R.T. Krause, FDA, Washington

1. Ethylenethiourea

Ethylenethiourea (ETU)7013

Column: Hypersil GOLD, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: H2O

B: ACNIsocratic: 60:40Flow Rate: 1 mL/minDetection: UV at 254 nmTemperature: 25 °C1. Tebuthiuron 4. Chlortoluron2. Monuron 5. Diuron3. Metoxuron 6. Linuron

Uron HerbicidesH250-051

Applications



B: 5 mM KH2PO4

Gradient: Time (min) %B0 952 956 7025 20

Flow Rate: 1 mL/minDetection: UV at 210 nmSource: Data Courtesy of M.C. Hennion,

ESPCI, France

1. Hydroxy-deisopropylatrazine 5. Hydroxyatrazine2. Diethyl-deisopropylatrazine 6. Deethylatrazine3. Hydroxy-deethylatrazine 7. Simazine4. Deisopropylatrazine 8. Atrazine

Degradation Productsof Atrazine

7043

Column: Hypersil GOLD C8™, 5 µm, 150 x 4.6 mm

Part Number: 25205-154630Mobile Phase: A: 0.1% Formic acid in MeOH

B: 0.1% Formic acid in H2OIsocratic: 50:50Flow Rate: 1 mL/minDetection: UV at 220 nmTemperature: 25 °C

1. p-Hydroxybenzaldehyde 4. Benzoic Acid2. Benzyl Alcohol 5. Nitrobenzene3. Impurity 6. Benzene

Contaminants in SoilH252-001

Column: Hypersil GOLD CN, 5 µm, 150 x 4.6 mm

Part Number: 25805-154630Mobile Phase: A: H2O + 0.1% Formic acid


1. Benzyl Alcohol 4. Toluene2. p-Hydroxybenzaldehyde 5. Ethyl Benzene3. o-Cresol

Contaminants in SoilH258-001

Column: Hypercarb, 5 µm, 100 x 4.6 mmPart Number: 35005-104630Mobile Phase: A: ACN + 1% TFA

B: H2O + 1% TFAIsocratic: 85:15Flow Rate: 1 mL/minDetection: UV at 254 nmTemperature: 40 °CSource: A. Gravel, National Rivers

Authority, Llanelli, UK

Phenoxy Acids 7039

1. Solvent2. Bentazone3. Dicamba4. MCPP

5. MCPA6. 2,4-D7. MCPB8. 2,4-DB

9. Benazolin10. Fluroxypyr11. 2,4,5,-T

Environmental


CarbamatesColumn: Hypersil GOLD™, 5 µm,

150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: H2O

B: MeOH Gradient: Time (min) % B

0 255 25

20 5530 90


1. Oxamyl 6. Carbofuran2. Methomyl 7. Carbaryl3. Hydroxy carbofuran 8. Naphthol4. Aldicarb 9. Methiocarb5. Propoxur

H250-095

260R011PAHsColumn: TR-50MS, 30 m x 0.25 mm x

0.25 µmPart Number: 260R142PTemperature: 50 °C 1 min, 8 °C/min to 300 °C,

hold 10 minDetector Type: MSCarrrier Gas: He 20 psiInjection Mode: Split 40:1, 300 °C

1. Naphthalene 9. Chrysene2. Acenaphthylene 10. Benzo (a) anthracene3. Acenaphthene 11. Benzo (b) Fluoranthene4. Fluorene 12. Benzo (k) Fluoranthene5. Phenanthrene 13. Benzo (a) pyrene6. Anthracene 14. Indeno (1,2,3-cd) pyrene7. Pyrene 15. Dibenzo (ah) anthracene8. Fluorathene 16. Benzo (ghi) perylene

Quadrupole GC/MSAnalysis ofPolybrominatedDiphenyl Ethers (PBDE) inEnvironmental SamplesColumn: TR-5MS,15m x 0.25 mm x 0.1 µmPart Number: 260F035PTemperature: 80 °C 5 min, 20 °C/min to 225 °C,

hold 5 minDetector Type: MS DSQ™

Carrier Gas: HeInjection Mode: Cold on-column

1. Tri-BDE (28) 6. Hexa-BDE (154)2. Tetra-BDE (47) 7. Hepta-BDE (183)3. Penta-BDE (99) 8. Octa-BDE (205)4. Penta-BDE (100) 9. Nona-BDE (206)5. Hexa-BDE (153) 10. Deca-BDE (209)

AN10147

Applications


Minnesota Ag ListPesticides Mix BColumn: TR-35MS, 30 m x 0.25 mm

x 0.25 µmPart Number: 260C142PInitial Temp: 100 °C, 1 minRate 1: 15 °C/min to 250 °CFinal Temp: 250 °C, 5 minDetector Type: MSDetection TRACE DSQ™ MS, source 225 °C, Conditions: 50-650 m/z, EI @ 70 eVCarrier Gas: HeFlow Rate: 1 mL/minInjection Mode: PTV split at 250 °CSplit Ratio 20:1

1. EPTC2. Phorate3. Terbufos4. Triallate5. Fonofos6. Chlorpyrifos

06040501

Minnesota Ag ListPesticides Mix AColumn: TR-35MS, 30 m x 0.25 mm

x 0.25 µmPart Number: 260C142PInitial Temp: 100 °C, 1 minRate 1: 15 °C/min to 250 °C,Final Temp: 250 °C, 5 minDetector Type: MSDetection TRACE DSQ MS, source 225 °C, Conditions: 50-650 m/z, EI @ 70 eVCarrier Gas: HeFlow Rate: 1 mL/minInjection Mode: PTV, Split at 250 °CSplit Ratio: 20:1

1. Ethalfluralin 9. Simazine2. Tifluralin 10. Acetochlor3. Propachlor 11. Dimethenamid4. Atrazine-desethyl 12. Alachlor5. Atrazine-desisopropyl 13. Metribuzin6. Prometon 14. Metolachlor7. Propazine 15. Pendimethalin8. Atrazine 16. Cyanazine

06040505


Environmental


Minnesota Ag ListPesticides Mix BColumn: TR-5MS, 15 m x 0.25 mm

x 0.25 µmPart Number: 260F130PInitial Temp: 100 °C, 1 minRate 1: 15 °C/min to 250 °CFinal Temp: 250 °C, 5 minDetector Type: MSDetection PolarisQ ™, source 225 °C, Conditions: 35-500 m/z, EI @ 70 eVCarrier Gas: HeFlow Rate: 1 mL/minInjection Mode: PTV split, 20 °CSplit Ratio: 90:1

06040506

Automated Cold-on-ColumnInjection and the Analysisof Explosive Residues byNegative ChemicalIonization GC/MSColumn: TR-8095, 12 m x 0.32 mm

x 0.25 µmPart Number: 260P123PTemperature: 80 °C 5 min, 20 °C/min

to 225 °C, hold 5 minDetector Type: MS DSQCarrier Gas: HeInjection Mode: Cold on-column

1. 2,6-dinitrotoluene 6. 4-amino-2,6-dinitrotoluene2. 1,3-dinitrobenzene 7. RDX3. 2,4-dinitrotoluene 8. 2-amino-4,6-dinitrotoluene4. 2,4,6-trinitrotoluene 9. Tetryl5. 1,3,5-trinitrobenzene 10. HMX

AN10130

Synthetic PyrethroidsColumn: TR-50MS, 30 m x 0.25 mm x 0.25 µmPart Number: 260R142PTemperature: 50 °C 1 min, 30 °C/min to 200 °C,

4 °C/min to 300 °C, hold 5 minDetector Type: MSCarrrier Gas: He, 6.8 psiFlow Rate: 1 mL/minInjection Volume: 1 µLInjection Mode: Splitless, 0.5 minInjection Temperature: 250 °C

1. EPTC2. Phorate3. Terbufos

4. Fonofos5. Triallate6. Chlorpyrifos

1. Natural Pyrethrums2. BHT3. Allethrin4. Bifenthrin5. Bioresmethrin6. Resmethrin7. Fenpropathrin8. Sumithrin9. Tetramethrin

10. Permethrin11. Cyfluthrin12. Flucythrinate13. Cypermethrin14. Esfenvalerate15. Fenvalerate16. Tralomethrin17. Deltamethrin

260R012

Applications


OrganochlorinePesticidesColumn: TR-5MS, 30 m x 0.25 mm

x 0.5 µmPart Number: 260F223PTemperature: 40 °C 1 min, 30 °C/min to

190 °C for 3 min, 10 °C/min to300 °C, hold 5 min

Detector Type: FIDCarrier Gas: HeInjection Details: Splitless

20075a

Minnesota Ag ListPesticides Mix AColumn: TR-5MS, 15 m x 0.25 mm

x 0.25 µmPart Number: 260F130PInitial Temp: 100 °C, 1 minRate 1: 15 °C/min to 250 °CFinal Temp: 250 °C, 5 minDetector Type: MSDetection PolarisQ, source 225 °C, Conditions: 35-500 m/z, EI @ 70 eVCarrier Gas: HeFlow Rate: 1 mL/minInjection Mode: PTV splitSplit Ratio: 90:1, 200 °C

1. Propachlor 9. Propazine2. Ethalfluralin 10. Dimethenamid3. Trifluralin 11. Acetochlor4. Atrazine-deisopropyl 12. Alachlor5. Atrazine-desethyl 13. Metolachlor6. Prometon 14. Cyanazine7. Simazine 15. Pendimethalin8. Atrazine

06040507

1. 2,4,5,6 - tetrachloro-meta-xylene 12. p,p-DDE2. α-BHC 13. Dieldrin3. β-BHC 14. Endrin4. γ-BHC 15. p,p-DDD5. δ-BHC 16. Endosulfan B6. Heptachlor 17. Endrin Aldehyde7. Aldrin 18. p,p-DDT8. Heptachlorepoxy 19. Endosulfan Sulfate9. γ-chlordane 20. Methoxychlor10. α-chlordane 21. Endrin Ketone11. Endosulfan A 22. Decachlorobiphenyl


Environmental


Column: TR-5, 15 m x 0.53 mm x 1 µmPart Number: 260E286PTemperature: 85 °C, 10 °C/min to 195 °CDetector Type: FIDInjection Details: Split

1. Chlorobenzene 5. Hexachlorobutadiene2. 1,2-Dichlorobenzene 6. Hexachlorocyclopentadiene3. 1,3-Dichlorobenzene 7. 2-Chloronaphthalene4. Hexachloroethane 8. Hexachlorobenzene

ChlorinatedHydrocarbons

EPA 609 Nitro Aromatics

20074b

Column: TR-WAX, 30 m x 0.53 mm x 1 µm Part Number: 260W298PTemperature: 80 °C, 10 °C/min to 160 °CDetector Type: FIDInjection Mode: Split

1. Benzene2. Toluene3. Ethylbenzene4. Chlorobenzene5. 1,3-Dichlorobenzene6. 1,4-Dichlorobenzene7. 1,2-Dichlorobenzene

260W011

EPA 602 Aromatics

KetonesColumn: TR-WaxMS, 30 m x 0.25 mm

x 0.25 µmPart Number: 260X142PTemperature: 40 °C 5 min, 10 °C/min to 190 °CDetector Type: MSCarrrier Gas: He 25 psiFlow Rate: 1.6 mL/minInjection 0.5 µLVolume:Injection Mode: Split 80:1, 250 °C

260X018

1. Acetone2. 2-Butanone3. 2-Pentanone4. 3-Pentanone5. 4-Methyl-2-pentanone6. 3-Methyl-2-pentanone7. 3-Hexanone8. 2-Methyl-3-hexanone9. 2-Hexanone10. 4-Methyl-2-hexanone11. Mesityl oxide

12. 5-Methyl-2-hexanone13. 3-Heptanone14. Cyclopentanone15. 2-Heptanone16. Cyclohexanone17. Octanone18. 2-Nonanone19. 2-Decanone20. 2-Undecanone21. 2-Dodecanone

Column: TR-WAX, 30 m x 0.53 mm x 1 µm Part Number: 260W298PTemperature: 190 °C, 15 °C/min to 240 °C,

hold 3 minDetector Type: FIDInjection Mode: Split

1. Nitrobenzene2. Isophorone3. 2,6-Dinitrotoluene4. 2,4-Dinitrotoluene

260W012

Applications


Phenol MixtureColumn: TR-35MS, 30 m x 0.25 mm

x 0.25 µmPart Number: 260C142PTemperature: 80 °C 1 min, 10 °C/min to 300 °C,

hold 5 minDetector Type: MSCarrrier Gas: He 29.2 psiFlow Rate: 1.7 mL/minInjection 1 µLVolume:Injection Mode: Split 100:1, 250 °C

1. Phenol 10. 3,5-Dimethylphenol2. 2-Chlorophenol 11. 2,4-Dichlorophenol3. o-Cresol 12. 2,3-Dimethylphenol4. p-Cresol 13. Isopropylphenol5. m-cresol 14. 4-Chloro-3-methylphenol6. 2,5-dimethylphenol 15. 2,4,6-Trichlorophenol7. 2,4-Dimethylphenol 16. 4-Nitrophenol8. 2-Nitrophenol 17. 4,6-Dinitrocresol9. p-Ethylphenol

24060502

EPA 625 Phenols (5 ng)Column: TR-5MS, 30 m x 0.25 mm x 0.25 µmPart Number: 260F142PTemperature: 40 °C 1 min, 8 °C/min to 360 °CDetector Type: FIDCarrrier Gas: H2, 12 psiInjection Mode: Split, 380 °C

1. Phenol2. 2-Chlorophenol3. 2-Nitrophenol4. 2,4-Dimethylphenol5. 2,4-Dichlorophenol6. 4-Chloro-3-methylphenol7. 2,4,6-Trichlorophenol8. 2,4-Dinitrophenol9. 4-Nitrophenol10. 2-Methyl-4,6-dinitrophenol11. Pentachlorophenol

260F015

Aromatic PollutantsColumn: TR-WaxMS, 30 m x 0.25 mm

x 0.25 µmPart Number: 260X142PTemperature: 60 °C Isothermal 10 minDetector Type: FIDCarrrier Gas: He 17.3 psiFlow Rate: 1.5 mL/minInjection 0.2 µLVolume:Injection Mode: Split 100:1, 250 °C

1. Benzene2. Toluene3. Ethyl benzene4. p-Xylene5. m-Xylene6. o-Xylene

260X019

Environmental


260R013Pesticides and HerbicidesColumn: TR-50MS, 30 m x 0.25 mm

x 0.25 µmPart Number: 260R142PTemperature: 50 °C 1 min, 70 °C/min to 190 °C,

4 °C/min to 280 °C, hold 5 minDetector Type: MSCarrrier Gas: He 20 psiInjection 1 µLVolume:Injection Mode: Splitless, 1 min

1. Methyldymron decomp. I2. Methyldymron decomp. II3. Trichlorofon (DEP)4. Etridiazole5. Chloroneb6. Benfluralin7. Pencycuron8. Simazine (CAT)9. Diazinon10. Propyzamide11. Chlorothalonil (TPN)12. Terbucarb (MBPMC)13. Tolclofos14. Fenitrothion (MEP)

15. Chlorpyrifos16. Pendimethalin17. Isophenphos18. Methyldymrom19. Captan20. Butamifos21. Napropamide22. Flotolanil23. Isoprothiolane24. Isoxathion25. Mepronil26. Pyridaphenthion27. Iprodione

260R014EPA 8081 OrganochlorinePesticidesColumn: TR-50MS, 30 m x 0.25 mm


8 °C/min to 320 °CDetector Type: MSCarrrier Gas: He Flow Rate: 35cm/sInjection 1 µLVolume:Injection Mode: Split 40:1, 280 °C

1. α-BHC2. γ-BHC3. β-BHC4. Heptachlor5. δ-BHC6. Aldrin7. Heptachlorepoxy8. trans-Chlordane9. cis-Chlordane10. Endosulfan A

11. p,p'-DDE12. Dieldrin13. Endrin14. p,p'-DDD15. Endosulfan B16. p,p'-DDT17. Endrin aldehyde18. Endosulfan sulfate19. Methoxychlor20. Endrin ketone


Applications


EPA 624 Purgeables in Drinking WaterColumn: TR-V1, 30 m x 0.25 mm x 1.4 µm Part Number: 260V332PTemperature: 50 °C 2 min, 15 °C/min to 170°CDetector Type: MSCarrrier Gas: He 15 psi

1. 1,1-Dichloromethane2. Dichloromethane3. cis-1,2-Dichloroethylene4. Chloroform5. 1,1,1-Trichloroethane6. Carbon tetrachloride7. 1,2-Dichloroethane8. Benzene9. Trichloroethylene10. Bromodichloromethane11. cis-1,3-Dichloropropene12. trans-1,3-Dichloropropene13. 1,1,2-Trichloroethane14. Tetrachloroethylene15. Dibromochloromethane16. Bromoform

260V010

260F014EPA 608.1OrganochlorinePesticidesColumn: TR-5MS, 30 m x 0.25 mm x 0.25 µm Part Number: 260F142PTemperature: 50 °C 1 min, 30 °C/min to 150 °C,

6 °C/min to 260 °CDetector Type: MSCarrrier Gas: He Flow Rate: 30 cm/sInjection 1 µLVolume:Injection Mode: Splitless 0.5 min

1. DBCP2. Etradiazole3. Chloroneb4. Propachlor5. PCNB6. Chlorobenzylate7. Chloropropylate

260R010EPA 625Column: TR-50MS, 30 m x 0.25 mm


hold 10 minDetector Type: MSInjection Mode: Split 40:1

1. 2-Chlorophenol2. 2-Nitrophenol3. 2, 4-Dimethylphenol4. 2, 4-Dichlorophenol5. 4-Chloro-3-methylphenol6. 2, 4, 6-Trichlorophenol7. 2, 4- Dinitrophenol8. 4-Nitrophenol9. 2-Methyl-4, 6-dinitrophenol10. Pentachlorophenol

Environmental


260C012EPA 608 OrganochlorinePesticidesColumn: TR-35MS, 30 m x 0.25 mm

x 0.25 µm Part Number: 260C142PTemperature: 130 °C 2 min, 10 °C/min to 320 °CDetector Type: MSCarrrier Gas: He Flow Rate: 30 cm/sInjection 1 µLVolume:Injection Mode: Split 40:1

1. α-BHC2. γ-BHC3. β-BHC4. Heptachlor5. δ-BHC6. Aldrin7. Heptachlor Epoxide (isomer B)8. Endosulfan I9. 4,4'-DDE

10. Dieldrin11. Endrin12. 4,4'-DDD13. Endosulfan II14. 4,4'-DDT15. Endrin aldehyde16. Endosulfan sulfate17. Methoxychlor18. Endrin ketone

EPA 624 PurgeablesColumn: TR-WaxMS, 30 m x 0.25 mm

x 0.25 µmPart Number: 260X142PTemperature: 32 °C 3 min, 8 °C/min to 90 °C,

6 °C/min to 200 °C, hold 5 minDetector Type: MSCarrrier Gas: He 27.2 psi, 35cm/sFlow Rate: 1.8 mL/minInjection 0.5 µLVolume:Injection Mode: Split 40:1, 250 °C

260X020

1. Chloromethane2. Vinyl chloride3. Trichlorofluoromethane4. Chloroethane5. Bromomethane6. 1,1-Dichloroethene7. Unknown8. trans-1,2-Dichloroethene 9. Carbon tetrachloride10. 1,1,1-Trichloroethane11. 1,1,-Dichloroethane12. Chloroform under methanol13. Dichloromethane14. Benzene15. Trichloroethene16. Tetrachloroethene

17. Toluene18. 1,2-Dichloropropane19. 1,2-Dichloroethane20. Ethylbenzene21. 1,3-Dichloropropene (Z)22. Bromodichloromethane23. 1,3-Dichloropropene (E)24. Chlorobenzene25. 1,1,2-Trichloroethane26. Dibromochloromethane27. 2-Chloroethylvinyl ether28. 1,3-Dichlorobenzene29. Tribromomethane30. 1,4-Dichlorobenzene31. 1,2-Dichlorobenzene32. 1,1,2,2-Tetrachloroethane


Nandrolone AnalysisAs steroid use becomes more complex, doping control agencies need a highly sensitive, discriminatory tool to detect these drugs. Hypersil GOLD columns provide symmetrical peakshapes leading to enhanced sensitivity and separation of structurally similar steroids.

The use of anabolic and androgenic steroids by athletes help them toincrease muscle mass and improve athletic performance. Steroid use isbanned in competitive sport, and doping control laboratories regularlytest competitors at all levels, both at competitions and in trainingsessions, to ensure they are not gaining an unfair advantage over others by chemically assisting their performance.

At large sporting events, the number of samples submitted isvery large. Both the testing laboratories and sports governing bodiesare under a great deal of pressure to detect banned drugs, such asnandrolone, as quickly and efficiently as possible. Since many steroidsdo not remain in the body in an unchanged format, the testing labora-tories also need to detect analytes resulting from the degradation ofthe original parent drug, or produced by the action of the parent drugon other biological analytes. These secondary analytes are often struc-turally similar to the parent drug.

High sample throughput of structurally similar compoundsrequires a column chemistry that can easily resolve individual analytesand generate sharp, symmetrical peaks for ultimate quantificationconfidence. An important requirement of the analytical method is itssensitivity. Athletes who do not want to be caught taking perform-ance-enhancing drugs will often cease taking the drugs for a periodof time before competition to allow the drug to leave their bodies.Often, trace levels of the drug will still be present after this time.Using a column that offers enhanced resolution and sensitivity providesgreater opportunity for drug detection.


Column: Hypersil GOLD™ 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: H2O


Results and DiscussionThe chromatogram shown in Figure 1 demonstrates the fast analysisof steroids. The run time of less than 5 minutes using isocratic conditions allows rapid sample turnaround and helps reduce overallanalysis cost. Hypersil GOLD’s ultra-pure base silica and state-of-the-art bonding generate highly symmetrical peaks, and allow structurallysimilar analytes to be positively differentiated from each other,decreasing the risk of inaccurate peak identification, and increasingpeak height, both of which improve the confidence in the method.

Figure 1: Separation of four testosterones, including nandrolone, in less than 5 minutes.

1. 11-Ketotestosterone 2. 19-Nortestosterone (Nandrolone)

3. Testosterone 4. Epitestosterone

H250-052

Analytes:

Applications


HPLC Analysis of FOX-7 using a Porous Graphitic Carbon ColumnThe strong retention properties of porous graphitic carbon (PGC) for very polar analytes were used to retain and analyse FOX-7 (2,2-dinitro-ethene-1,1-diamine) with HPLC.

The explosive FOX-7 is an extremely polar compound which is verydifficult to retain in conventional reversed phase conditions withoutthe addition of an ion pair reagent. When using a C18 column understandard conditions FOX-7 elutes with the solvent front.1

PGC is a material that provides strong retention of very polarcompounds. The retention mechanism involves a charge-inducedinteraction of the polar analyte with the polarizable surface of thegraphite.2 This so-called “polar retention effect on graphite” (PREG)can be controlled by the use of electronic modifiers, which competewith the polar analytes to the surface of the graphite reducing retention.3 In this application note the retention of FOX-7 is demonstratedon PGC using a mobile phase containing an electronic modifier, eitherTFA or ammonia.


Column: Hypercarb™ 5 µm, 100 x 3 mmPart Number: 35005-103030Mobile Phase: A1: H2O + 1% TFA

A2: H2O + 1% NH3B1: ACN + 1% TFAB2: ACN/ H2O/ NH3 (96:3:1)

Gradient: Time (min) % B (B1 or B2)0 03 07 100

24 100Flow Rate: 0.8 mL/minInjection Volume: 10 µLDetection: UV at 278 or 272 nm

Results and DiscussionDue to the PREG, FOX-7 did not elute with an acceptable retentioneven when a strong organic eluent such as acetonitrile was used.When 1% trifluoroacetic acid (TFA) was added to the mobile phase,as a competitive electronic modifier, the polar retention was reducedand the analyte eluted at 14 minutes with good peak shape (Figure1a). The suppression of polar interaction was also possible using abasic modifier, ammonia (NH3) in the mobile phase, in which case theretention time was 11 minutes (Figure 1b). This methodology wassuccessfully applied to the analysis of possible by-products in thesynthesis of FOX-7.1

References1. E. Holmgren, P. Goede, N. Latypov, C. Crescenzi, H. Carlsson, Poster 20012. P. Ross, LCGC Europe, May 20003. J. Knox, P. Ross, Advances in Chromatography, 1997, vol. 37, pp 120 –161

(Data courtesy of C. Crescenzi and H. Carlsson, Univ. of Stockholm, Sweden)

Figure 1: Retention of FOX-7 on PGC using an acidic (TFA) or basic (NH3) electronic modifier.

(a)

(b)

1. 2,2-dinitro-ethene-1,1-diamine

Analytes:

H350-1094

Forensics/Toxicology


GC/MS Analysis of Performance Enhancing Drugs in RacehorsesConventional GC/MS methods for the analysis of performance enhancing drugs in racehorses can be made faster while maintaining chromatographic integrity.

Horse racing worldwide is a multi-billion dollar industry and there canbe substantial rewards for winning. The horse racing testing laboratoriesaround the world form the defense against doping to ensure races arefair and horses are safe and healthy. As the requirement for checkingperformance enhancing drugs in race horses increases, throughputand analysis time become an important consideration in methoddevelopment.

This application note looks at method options to reduce analysistime while maintaining chromatographic parameters such as resolutionand selectivity. As an illustration, a GC/MS method for a standarddoping drugs test mixture was developed using a 0.25 mm internaldiameter (ID) TRACE TR-5MS column. This column showed good separation of nine compounds in approximately 22 minutes. Themethod was then transferred to a shorter, narrower bore column toreduce the time required for analysis.

Experimental ConditionsOriginal GC/MS Method (a)

Instrument: TRACE DSQ™ GC/MS systemColumn: TRACE™ TR-5MS, 30 m x 0.25 mm x 0.25 µmPart number: 260F142PInitial Temp.: 75 °C for 2 minRate 1: 15 °C/min to 300 °C Rate 2: 20 °C/min to 320 °C, hold 8 minCarrier Gas: He Flow Rate: 1.5 mL/minInjection Volume: 1 µL SplitlessDetection: MS

Fast GC/MS Method (b)

Instrument: TRACE DSQ GC/MS systemColumn: TRACE TR-5MS, 15 m x 0.15 mm x 0.25 µmPart Number: 260F128PInitial Temp.: 45 °C for 1 minRate 1: 100 °C/min to 200 °C Rate 2: 30 °C/min to 350 °C, hold 2 minCarrier Gas: He Flow Rate: 0.8 mL/minInjection Volume: 1 µL SplitlessDetection: MS

Results and DiscussionThe time required for the separation of nine doping drugs was successfully reduced by two-thirds by decreasing the GC columnlength from 30 to 15 m, the column ID from 0.25 to 0.15 mm, and bymaking the temperature program faster. In transferring methods toachieve a faster analysis time without changing elution order, the oneparameter that must not change is the phase of the column. The chromatograms in Figure 1 demonstrate that the selectivity and resolution were unaffected by the new parameters. By optimizingthese parameters the total analysis time for this range of drugs wasreduced from 22 (Figure 1a) to approximately 7 minutes (Figure 1b).This increase in speed can have a great effect on the throughputcapability of the lab and the productivity of the instruments.

Figure 1: The analysis time of drugs in race horses is drastically reduced fromover 22 min with a 30 m column (a) to about 7 min by using a shorter 15 m TR-5MS column (b).

Analytes: 1. Metronidazole; 2. Amylobarbitone; 3. Pentobarbitone; 4. Caffeine; 5. Diphenhydramine; 6. Trimipramine; 7. Phenytoin; 8. Diazepam; 9. Nordiazepam; 10. Diphenoxylate.

260F107

15070501

(a)

(b)

Applications





Benzodiazepinesfrom SerumCompounds: BenzodiazepinesPart Number: 60108-302Phase: HyperSep C18Volume: 1 mLBed Weight: 100 mgSample Mix 500 µL serum with 100 µL Pretreatment: 0.1 M sodium carbonate solution.

Add internal standard if requiredConditioning: 2 mL methanol followed by 2 mL

distilled waterApplication: Force or aspirate sample slowly

through columnWashing: 2 mL distilled water followed by

50 µL methanolElution: 2 x 200 µL volumes methanol

Carboxy Δ9Tetrahydrocannibinol(THC) in UrineCompounds: Carboxy Δ9 THCPart Number: 60108-304Phase: HyperSep™ C18Volume: 3 mLBed Weight: 500 mgSample To 5 mL urine add 0.5 mL 10N KOHPretreatment: Heat at 55 °C for 15 min and then

cool. Add 1 mL glacial acetic acid.Conditioning: 6 mL methanol followed by 6 mL

0.01N HClApplication: Force or aspirate sample slowly

through columnWashing: 2 x 500 µL volumes acetonitrile/

0.01N HCl (60:40, v/v). Evaporateto dryness under vacuum

Elution: 2 x 500 µL volumes n-heptane/ethylacetate (85:15, v/v)

Amphetamines, Opiatesand Phencyclidine in Oral FluidCompounds: Amphetamines, opiates,

phencyclidinePart Number: 60108-741Phase: HyperSep Verify™-CXVolume: 1 mLBed Weight: 50 mgSample Add 100-500 µL neat sample to aPretreatment: clean tube. Add internal standard

and leave for 10 min at ambient temperature. Add 800 µL 100 mMphosphate buffer pH 6 Mix/vortexfor 10 sec. Use 100 mM monoba-sic or dibasic sodium phosphateto ensure pH 6.

Conditioning: 200 µL CH3OH200 µL deionized water200 µL 100 mM phosphate buffer pH 6

Application: Do not exceed 1 mL/minWashing: 500 µL deionized water

500 µL 100 mM acetic acid500 µL CH3OH. Dry column

Elution: 800 µL CH2Cl2/IPA/NH4OH (70:26:4)Do not exceed 1 mL/minPrepare elution solvent daily

Amphetamines in UrineCompounds: AmphetaminesPart Number: 60108-742Phase: HyperSep Verify-CXVolume: 10 mLBed Weight: 200 mgSample To 2 mL urine add internal Pretreatment: standard(s), 1 mL 100 mM

phosphate buffer pH 6 and 1 mL0.35 M sodium periodate.Mix/vortex and incubate at ambient temperature for 20 min.Use 100 mM monobasic or dibasicsodium phosphate to ensure sample pH of 6.0±0.5.

Conditioning: 3 mL CH3OH followed by 3 mL deionised water and 1 mL 100 mMphosphate buffer (pH 6)Aspirate at < 3 inches Hg to prevent sorbent drying

Application: Load at 1 to 2 mL/minWashing: 3 mL deionized water followed by

1 mL 100 mM acetic acid and 3 mL CH3OH. Dry column (5 min at >10 inches Hg)

Elution: 3 mL CH2Cl2/IPA/NH4OH (78:20:2)Collect eluate at 1 to 2 mL/minPrepare elution solvent dailyConcentrate eluate by adding 30 µLsilation grade DMF to eluate. Evaporate to 30 µL at < 40 °C

Therapeutic and AbusedDrugs in Urine forAcid/Neutral and Basic DrugsCompounds: Barbiturates, ibuprofen, cotinine,

amphetamine, codeine, ketaminePart Number: 60108-742Phase: HyperSep Verify-CXVolume: 10 mLBed Weight: 200 mgSample To 2 mL urine add internal Pretreatment: standard(s) and 1 mL 100 mM

phosphate buffer (pH 6). Mix/vortex. Use 100 mM monobasic ordibasic sodium phosphate toensure sample pH of 6.

Conditioning: 3 mL CH3OH3 mL deionized water2 mL 100 mM phosphate buffer (pH 6)Aspirate at < 3 inches Hg

Application: Load at 1 to 2 mL/minWashing: 3 mL deionized water

1 mL 100 mM acetic acidDry column (5 min at >10 inches Hg) 2 mL hexane

Elution: Acidic and Neutral: 3 mLhexane/ethyl acetate (50:50)Collect eluate at < 2 mL/minEvaporate to dryness at < 40 °CBasic: 3 mL CH2Cl2/IPA/NH4OH (78:20:2). Collect eluate at 1-2 mL/min Evaporate to drynessat < 40 °C using evaporator


Applications


Drugs from Blood and UrineCompounds: Amphetamines, barbiturates,

opiatesPart Number: 60108-304Phase: HyperSep C18Volume: 3 mLBed Weight: 500 mgSample Adjust 10 mL urine to desired Pretreatment: pH value using HCI or ammonia

and centrifuge Amphetamines and Opiates: pH 8-9Active components: pH 7-8Barbiturates: pH 7

Conditioning: 6 mL methanol followed by 6 mL Distilled water pH7

Application: Force or aspirate sample slowly through column

Washing: 6 mL water. Dry column under vacuum for 5 min

Elution: Aspirate 750 µL eluent into column.Elute after 1 min and then flushwith 750 µL eluent. Eluents: Cannabinoids: acetone. Barbiturates, active components, bases, amphetamines: acetone/chloroform (1:1)

Abused Drugsin Equine UrineCompounds: Aminocaproic acid

(6-aminohexanoic acid)Part Number: 60108-421Phase: HyperSep SCXVolume: 1 mLBed Weight: 100 mgSample Mix 1 mL urine with 1 mL Pretreatment: phosphoric acid (7 mM). Use con-

centrated H3PO4 to adjust pH to 2Conditioning: 1 mL methanol followed by 1 mL

distilled water and 1 mL 7 mMH3PO4

Application: Force or aspirate sample slowly through column Dry column under vacuum for 30 sec

Washing: 1 mL 7 mM phosphoric acid0.5 mL 0.1 M acetic acid1 mL methanolDry column under vacuum for 30 sec

Elution: 2 x 1 mL ammoniacal methanol (1%)

Methadone in UrineCompounds: Methadone Part Number: 60108-742Phase: HyperSep™ Verify™-CXVolume: 10 mLBed Weight: 200 mgSample To 2 mL urine add internal Pretreatment: standard(s) and 1 mL 100 mM

phosphate buffer (pH 6). Mix/vortex.Use 100 mM monobasic or dibasic sodium phosphate toensure sample pH of 6.

Conditioning: 3 mL CH3OH3 mL deionized water2 mL 100 mM phosphate buffer (pH 6)Aspirate at < 3 inches Hg

Application: Load at 1 to 2 mL/minWashing: 3 mL deionized water

1 mL 100 mM acetic acid3 mL CH3OHDry column (5 min at >10 inches Hg)

Elution: 3 mL CH2Cl2/IPA/NH4OH (78:20:2)Collect eluate at 1-2 mL/minPrepare elution solvent daily

Column: Hypercarb, 7 µm, 100 x 4.6 mmPart Number: 35007-104630Mobile Phase: A: NH4OAc at pH 9.0

B: MeOHIsocratic: 40:60Flow Rate: 1 mL/minDetection: UV at 220 nmSource: R.D. Knaggs, D. Barrett and P.N.

Shaw, Nottingham University, UK.

1. Normorphine2. Morphine-3-glucuronide3. Morphine-6-glucuronide4. Morphine5. Codeine

Morphine andMetabolites

7047



1. Cloxazolam 5. Oxazepam2. Medazepam 6. Temazepam3. Nitrazepam 7. Nordiazepam4. Lorazepam 8. Diazepam

BenzodiazepinesH250-014


B: ACN + 0.1% TFAGradient: 0 % B for 3 min, then to 100% B

in 15 minFlow Rate: 0.2 mL/minDetection: ELSDSource: J-P. Mercier, Universite d’Orleans,

Orleans, France

Alkyl Phosphonic AcidsH350-1095

1. Methylphosphonic acid2. Ethylphosphonic acid3. 2-Methoxyethyl

methylphosphonic acid4. 2-Methoxyethyl

ethylphosphonic acid

5. Cyclopentyl methylphosphonic acid

6. Cyclohexyl methylphosphonic acid

7. Cyclohexyl ethylphosphonic acid





1. Chlorpromazine

ChlorpromazineH250-031



1. Promazine 3. Chlorpromazine2. Propionylpromazine 4. Triflupromazine

Anti-PsychoticsH250-032

Column: Hypersil GOLD™, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: H2O


1. 11-Ketotestosterone2. 19-Nortestosterone (nandrolone)3. Testosterone4. Epitestosterone

TestosteronesH250-052


B: ACN Gradient: 15-45% B in 20 minFlow Rate: 1.5 mL/minDetection: UV at 205 nmTemperature: 25 °C

1. 2-Ethyl-2-phenylmalonamide2. Primidone3. Phenobarbital4. Hexobarbital5. Carbamazepine6. 5,5-Dipenylhydantoin

AnticonvulsantsH250-080

Column: Hypersil GOLD, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: 25 mM NH4OAc pH 6


1. Nordoxepin2. Chlordiazepoxide3. Oxazepam

AnxiolyticsH250-072

Column: TR-5MS, 15 m x 0.25 mm x 0.25 µm

Part Number: 260F230PTemperature: 190 °C for 2 min, 40 °C/min

to 270 °CDetector: MSDetetcor TRACE DSQ™ MS sourceConditions: 250 °C using SIM modeCarrier Gas: HeFlow Rate: 2 mL/minInjection Details: Split 15:1 175 °C

20075b

Amphetamine andMethamphetamine

Applications


CannabinoidsColumn: Hypersil GOLD™, 1.9 µm,


B: ACNIsocratic: 33:67Flow Rate: 0.3 mL/minDetection: MS at TSQ Quantum™ Discovery™

MAX HESI +Temperature: AmbientSource: Robert Huls & Wim Van

Duinkerken, Thermo FisherScientific, NL

1. Cannabidiol acid 5. Cannabinol2. Cannabigerol acid 6. Δ-9-Tetrahydrocannabinol3. Cannabigerol 7. Cannabichromene4. Cannabidiol 8. Δ-9-Tetrahydrocannabinol acid

H250-083

AlkaloidsColumn: Hypersil GOLD aQ™, 5 µm,

150 x 4.6 mmPart Number: 25305-154630Mobile Phase: A: 50 mM NaH2PO4, pH 2.0


1. Nicotine2. Anabasine3. Cotinine

H253-006

1

2

3

1

2

3 & 4

5

6 78

Tricyclic AntidepressantsColumn: Hypersil GOLD, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: 0.1% Formic acid


Concentration: 2.5 ng/µL 1. Doxepin2. Protriptyline3. Imipramine4. Nortriptyline5. Amitriptyline6. Trimipramine

H250-050





B: ACN:2-Propanol (1:3) + 0.1% TFA

Gradient: 5 to 100% B in 10 minFlow Rate: 1 mL/minDetection: UV at 225 nmTemperature: 25 °C

1. 2-Methylhippuric acid2. Hippuric acid3. 3-Methylhippuric acid4. 4-Methylhippuric acid

Hippuric Acid IsomersH350-1023

0 5 10 MIN

1

2

34

Column: Hypercarb, 5 µm, 100 x 3.0 mmPart Number: 35003-103030Mobile Phase: A: H2O + 1% TFA or 1% NH3 (aq)

B: ACN + 1% TFA orACN:H2O:NH3 (96:3:1)

Gradient: 0% B for 3 min; 0 to 100% B in 7 min

Flow Rate: 0.8 mL/minDetection: UV at 278 or 272 nmSource: C. Crescenzi and H. Carlsson,

Univ. of Stockholm, Sweden

1. 2,2 Dinitro-ethene-1, 1-diamine

H350-1094

FOX 7




1. Nicotine

NicotineH250-049

Column: Hypercarb, 7 µm, 100 x 4.6 mmPart Number: 35007-104630Mobile Phase: 2.5 mM L-ZGP + 1.5 mM NaOH

in ACN:MeOHIsocratic: 94:6Flow Rate: 1 mL/minDetection: UV at 275 nmSource: A. Karlsson, Astra Hässle AB,

Sweden

1. Trimipramine 2. Promethazine

Trimipramine andPromethazine

7056

1

1

Applications


Amytriptyline and NortriptylineColumn: TR-35MS, 30 m x 0.25 mm

x 0.25 µmPart Number: 260C142PInitial Temp: 100 °C, 0.2 minRate 1: 30 °C/min to 300 °CFinal Temp: 300 °C, 0.5 minDetector Type: MSDetection TRACE DSQ MS, source Conditions: 225 °C, 50-400 m/z, EI @ 70 eVCarrier Gas: HeFlow Rate: 1 mL/minInjection Temp: 250 °CInjection Mode: Split Split Ratio: 10:1

1. Amytriptyline2. Nortriptyline

06040504

Barbiturates(underivatized)Column: TR-35MS, 30 m x 0.25 mm

x 0.25 µmPart Number: 260C142PInitial Temp: 150 °C, 0.2 minRate 1: 20 °C/min to 300 °CFinal Temp: 300 °C, 0.5 minDetector Type: MSDetection TRACE DSQ MS, source Conditions: 225 °C, 35-400 m/z, EI @ 70 eVCarrier Gas: HeFlow Rate: 1.5 mL/minInjection Temp: 250 °CInjection Mode: Split Split Ratio: 50:1

1. Pentabarbital 3. Hexabarbital2. Secobarbital 4. Phenobarbital

11040502

Drugs of Abuse (underivatized)Column: TR-5MS, 15 m x 0.25 mm

x 0.25 µmPart Number: 260F142PInitial Temp: 150 °C, 0.2 minRate 1: 20 °C/min to 300 °CFinal Temp: 300 °C, 0.5 minDetector Type: MSDetection PolarisQ ™ source 225 °C, Conditions: 35-400 m/z, EI @ 70 eVCarrier Gas: HeFlow Rate: 1.5 mL/minInjection Temp: 250 °CInjection Details: Split Split Ratio: 50:1

1. Caffeine 5. Codeine2. Phencyclidine 6. 6-acetylmorphine3. Methadone 7. Heroin4. Cocaine

11040504

12

3

4

1

2

1

2

3 4

5

6

7



Drugs of Abuse(underivatized)Column: TR-35MS, 30 m x 0.25 mm

x 0.25 µmPart Number 260C142PInitial Temp: 150 °C, 0.2 minRate 1: 20 °C/min to 300 °CFinal Temp: 300 °C, 0.5 minDetector Type: MSDetection TRACE DSQ MS, source 225 °C, Conditions: 35-400 m/z, EI @ 70 eVCarrier Gas: HeFlow Rate: 1.5 mL/minInjection Temp: 200 °CInjection Details: Split Split Ratio: 80:1

1. Phencyclidine 5. Codeine2. Caffeine 6. 6-acetylmorphine3. Methadone 7. Heroin4. Cocaine

11040503

Antidepressant andAnticonvulsant DrugsColumn: TR-50MS, 30 m x 0.25 mm

x 0.25 µmPart Number: 260R142PTemperature: 150 °C 0.5 min, 10 °C/min to

180 °C, 1.5 °C/min to 220 °C, 30 °C/min to 260 °C, hold 5 min

Detector Type: MSCarrier Gas: He 25.7 psiFlow Rate: 1.8Injection Volume: 1.0 µLInjection Details: Splitless 0.5 min,

24060504

1

2

3

4

5 6 7

FentanylColumn: TR-35MS, 30 m x 0.25 mm

x 0.25 µmPart Number: 260C142PInitial Temp: 100 °C, 0.2 minRate1: 30 °C/min to 300 °CFinal Temp: 300 °C, 0.5 minDetector Type: MSDetection TRACE DSQ MS, source 225 °C,Conditions: 50-400 m/z, EI @ 70 eVCarrier Gas: HeFlow Rate: 1 mL/minInjection Details: split 10:1 at 250 °C

1. Fentanyl

06040503 1

1. Benzothiazole2. Selegeline3. Methsuximide4. Ketamine5. Unknown

6. Brompheniramine7. Impipramine8. Mianserin9. Diothiepin10. Marbamazepine

11. Prazepam12. Diltiazem13. Pholcodine

Applications


Barbiturates(underivatized)Column: TR-5MS, 15 m x 0.25 mm

x 0.25 µmPart Number: 260F130PInitial Temp: 150 °C, 0.2 minRate 1: 20 °C/min to 300 °CFinal Temp: 300 °C, 0.5 minDetector Type: MSDetection PolarisQ source 225 °C, Conditions: 35-400 m/z, EI @ 70 eVCarrier Gas: HeFlow Rate: 1.5 mL/minInjection Temp: 250 °CInjection Mode: Split Split Ratio: 20:1

1. Pentabarbital2. Secobarbital3. Hexabarbital4. Phenobarbital

11040505

1 2

3

4

Drugs in Horse UrineColumn: TR-5MS, 15 m x 0.15 mm x 0.25 µmPart Number: 260F128PTemperature: 45 °C, 200 °C/min to 200 °C,

30 °C/min to 350 °CDetector Type: MSCarrrier Gas: HeFlow Rate: 0.8 mL/minInjection 1 µLVolume:Injection Mode: 260 °C, splitless 0.8 min,

1. Metronidazole2. Amylobarbitone3. Pentobarbitone4. Caffeine5. Diphenhydramine6. Trimipramine7. Phenytoin8. Diazepam9. Nordiazepam10. Diphenoxylate

15070501




Basic DrugsColumn: TR-5MS, 25 m x 0.25 mm x

0.25 µmPart Number: 260F142PTemperature: 100 °C, 5 °C/min to 325 °C, then

hold 5 minDetector Type: FIDDetection: 380 °CCarrrier Gas: He 150 kPaInjection Mode: Split 20:1

1. Benzocaine2. Unknown3. Meperidine4. Diphenhydramine5. Lidocaine6. Tripelennamine7. Amitripyline8. Tetracaine9. Pyrilamine10. Unknown11. Diazepam12. Flurazepam13. Papaverine14. Triazolam

260F010

Drugs of Abuse in UrineColumn: TR-35MS, 25 m x 0.25 mm x

0.25 µmPart Number: 260C142PTemperature: 80 °C, 15 °C/min to 200 °C,

7 °C/min to 295 °C, 20 °C/min to340 °C, hold 6 min

Detector Type: FID

1. Cotinine2. Methadone3. Morphine-2AC4. 7-Amino-flunitrazepam-AC

260C011

Applications


Column: TR-5, 30 m x 0.53 mm x 1 µmPart Number: 260E298PTemperature: 200 °C, then 25 °C/min to 300 °CDetector Type: FIDInjection Mode: Split

1. Cocaine2. Codeine3. Morphine4. Quinine

260E010

Alkaloids

Column: TR-WAX, 30 m x 0.32 mm x 1 µmPart Number: 260W297PTemperature: 60 °C IsothermalDetector Type: FIDInjection Mode: Split

1. Acetone2. Ethyl Acetate3. Methanol4. iso-Propanol5. Ethanol6. n-Propanol

260W010

Blood Alcohols


Analysis of Aromatic Amines Produced by Degradation of Azo DyesHypersil GOLD columns generate highly symmetrical, narrow peaks to provide the ultimate sensitivity and quantification required for the accurate analysis of closely related,highly basic analytes.

Sixty-five percent of the organic colorants in use around the world areazo dyes.1 They provide intense, bright colors that are stable andhighly cost-effective due to the simple manufacturing methods. Theirmanufacture is also environmentally friendly as it takes place in water,so there is little solvent disposal or recycling required afterwards. Themajority of azo dyes are not considered dangerous; only about 5% areconsidered potentially hazardous because, under reduction conditions,they degrade to produce aromatic amines, a small number of which areclassified as being carcinogenic or potentially carcinogenic to humans.

New legislation by the European Commission to protect publichealth proposes that an amendment to Council Directive 76/769/EEC,“Marketing and Use of Azo Colorants” be made to restrict the use ofazo dyes.2,3 In order to protect human health, those azo dyes, whichcan break down under reductive conditions to release any of a groupof defined aromatic amines, are prohibited from being used in thoseconsumer goods that are considered to have regular skin contact(such as wristwatch straps, bed linen, textiles, toys etc). The EUDirective 2002/61/EC lists 22 aromatic amines which are banned andthus need to be monitored. The detectable amount of any aromaticamine should not exceed 30ppm in the finished articles or in the dyedparts thereof. Thus, sensitive and accurate analytical methods arerequired to monitor these aromatic amines.

The challenge for the chromatographic analysis of aromaticamines is that these are basic compounds with closely related struc-tures, occurring at low levels. Older type A and B, L1 bonded-phasesilica column chemistries have been used in the past to assay highlybasic amines but have required the addition of a competitive amine inthe mobile phase to obtain symmetrical peaks. Today, the accurateHPLC quantification of these amines requires an analytical columnthat can easily replace older L1-type columns in analytical methodswithout the requirement for excessive method revalidation and onethat can distinguish between structurally similar compounds and pro-vide highly symmetrical peaks.


Column: Hypersil GOLD™ 3 µm, 150 x 2.1 mmPart Number: 25003-152130Mobile Phase: A: 25 mM Ammonium acetate, pH 5

B: ACNGradient: 20 to 100% B in 10 min Flow Rate: 0.2 mL/minDetection: UV at 254 nmTemperature: 40 °C

Results and DiscussionThe chromatogram in Figure 1 demonstrates that the ultra-pure basesilica and state of the art bonding used for Hypersil GOLD media generate highly symmetrical peaks and allow very basic substances tobe positively differentiated from each other, increasing the confidencein analytical results and decreasing the risk to the consumer.

References1. Faversham House Group Ltd, 2002. Edie News Article2. Official Journal Of The European Union L 243, 11/09/2002, p 15 –183. Official Journal Of The European Union 57, 25/02/2004, p 4–5

Figure 1: Separation of six aromatic amines. Symmetrical peaks are obtainedwith a low concentration of a volatile buffer and a mobile phase gradient.

Analytes: 1. 2,2-diaminotoluene; 2. 4,4-oxydianiline; 3. o-toluidine; 4. 2-methoxy-5-methylaniline; 5. 2,4,5-trimethylaniline; 6. 4,4-methylene-bis(2-chloroaniline); 7. Unknown

H250-026

Industrial


GC Analysis of Biodiesel Using a High Temperature CarboraneModified Siloxane Phase ColumnA TRACE TR-HT5 high temperature stable GC column has been used to monitor the productionof biodiesel B100.

The manufacture of biodiesel involves the conversion of triglycerides(usually from vegetable oils) in the presence of an alcohol, to the corresponding ester. In this conversion, ethanol produces ethyl estersand methanol produces methyl esters. Methanol is the more commonlyused alcohol and rape seed oil (canola) is the most common startingmaterial. Biodiesel made from new rapeseed oil is referred to as RME(Rapeseed Methyl Esters), and that made from used cooking oil ofuncertain origin, is referred to as FAME (Fatty Acid Methyl Ester)biodiesel. After the reaction is complete, glycerol, a reaction by-product,and methanol (or ethanol) are removed as they adversely affect performance. The objective of the reaction is complete transesterifi-cation of the oil resulting in a fuel with a low viscosity, low flashpoint, low boiling point and with low concentrations of triglycerides.When used as a direct replacement for diesel, the fuel is referred toas biodiesel B100.

This application note demonstrates how a high temperature stable TRACE TR-HT5 column (5% phenylpolycarborane-siloxane) and the TRACE GC Ultra were used to monitor the conversion oftriglycerides to FAMEs for a production run of B100.1


SamplesSamples of B100 (from recycled vegetable oil) were obtained directlyfrom the manufacturer and derivatized according to ASTM methodD6584.2 References and internal standards are as specified in ASTMMethod D6584.2

GC Conditions

Instrument: TRACE GC Ultra™

Column: TRACE™ TR-HT5, 15 m x 0.25 mm x 0.1 µmPart Number: 260H035PInitial Temp.: 50 °C, hold 1 minRate 1: 15 °C/min. to 180 °C Rate 2: 7 °C/min. to 230 °CRate 3: 50 °C/min. to 365 °C, hold 10 minCarrier Gas: He Flow Rate: 3 mL/minPTV Injector: 50 °CRate 1: 14.5 °C/secFinal Temp.: 250 °C, hold 28 minSplit Ratio: 30:1Detector: FID (380 °C)

Results and DiscussionThe chromatograms obtained for the recycled vegetable oil startingmaterial and the biodiesel B100 final product, after removal of theglycerol and methanol, are shown in the Figure 1. The triglyceridesappear to be fully converted to esters by the end of the transesterifi-cation reaction. The biodiesel met the specification set is EN14214for both triglycerol and free glycerol.3

References1. J. Warden et al, poster presented at Pittcon 2007, Chicago, Feb 2007

(reference PO20374_E02/07)2. ASTM Standard D6584-003. European Standard EN 14214:2003

Figure 1: GC chromatograms for the starting material (recycled vegetable oil)and the B100 final product.

Applications


Characterization of High Boiling Components in Petroleum Productsusing Hypersil GOLD and LC/MSA fast and robust characterization of non- and semi-volatile components found in petroleumproducts is achieved, using a Hypersil GOLD 1.9 μm column and LC-MS.

The characterization of petroleum products is usually carried outusing GC and GC/MS due to the high volatility of a number of thecomponents. However, a significant portion of these products are highboiling or non/semi volatile and are difficult to analyze using GC/MSdue to volatilization or molecular weight limitations. LC/MS does notsuffer from such problems. Traditionally, however, such separationshave been marred by lengthy analysis times and hydrocarbon contam-ination of the MS interface. Now, using Hypersil GOLD 1.9 µm particlecolumns, together with a patented ‘cone wash’ integrated into theSurveyor MSQ Plus ESI source, a fast, uninterrupted and robust analysis is possible.

Experimental ConditionsInstruments

LC: Surveyor Plus™

MS: Surveyor MSQ Plus™

LC Conditions

Column: Hypersil GOLD™ 1.9 µm, 50 x 2.1 mmPart Number: 25002-052130Mobile Phase: A: H2O + 0.1% Formic acid

B: MeOH + 0.1% Formic acidGradient: 80% B to 100% B over 9 mins (Hold for 6 mins),

re-equilibration for 2 minsFlow Rate: 0.5 mL/minInjection Volume: 10 µLTemperature: 50 °C

MS Conditions

Mode: + ESIProbe Temp.: 550 °CCone Voltage: 75 VCone Wash: MeOH, 200 µL/min

Samples

Fuel System Cleaning Solutions, available commercially.

Dilutions: 10 µL of sample into 2 mL Hexane, followed by a 100 µLaliquot into 1 mL Hexane.

Results and DiscussionLC/MS analysis enables analysis of non- and semi-volatiles in petro-leum products over a wide mass range, including polymer as well aslow mass components. Use of Hypersil GOLD 1.9 µm particles pro-vides excellent resolution and efficiency for the sensitive analysis of petroleum products as well as enabling fast analysis times. TheMSQ Plus cone wash removes non-polar hydrocarbon components,eliminating system contamination and increasing reproducibility andmethod robustness.

References1. J. Huang et al.Poster presented at ASMS 2006.(Reference T018P_ASMS06).

Figure 1: Total Ion Chromatograms (a) and averaged mass spectra (3 to 15 min)for 2 samples (b). Example of a polymeric distribution series (c).

(a)

(b)

(c)

Industrial


Applications


Industrial

Column: TR-1, 30 m x 0.53 mm x 5 µmPart Number: 260A470PInitial Temp: Isothermal, 50 °CDetector: FIDCarrier Gas: HeInjection Volume: 1 µLInjection Mode: SplitSplit Ratio: 20:1, 300 °C

1. Methanol2. Ethanol

Ethanol Impurityin Methanol

23110401

Column: Hypersil GOLD5 µm, 150 x 4.6 mm

Part Number: 25005-154630Mobile Phase: A: 0.1% trifluoroacetic acid

B: acetonitrileGradient: 100%A for 5 min, then to 15%B

by 7.5 min, then to 39%BFlow Rate: 1.0 mL/minDetection: UV-VISTemperature: 25 °CSource: A Romieu, IRCOF,

University of Rouen

1. Symmetrical cyanine dye2. Asymmetrical cyanine dye

Cyanine DyesH250-102


B: H2O Isocratic: 10:90Flow Rate: 1 mL/minDetection: UV at 288 nmSource: Mr. Valleix, CEA Saclay,

« Laboratoire des MoléculesMarquées », France

1. 2,5-Dimethyl-4-hydroxy-3(2H)furanone2. 5-(Hydroxymethyl)furfural3. 3-Hydroxy-2-methyl-4-pyrone

Furanones, Furfuralsand Pyrones

05020302




1. 2,4,6-Trinitrotoluene 3. 4-Nitrotoluene2. 2,6-Dinitrotoluene

NitroaromaticsH254-003

Column: Hypercarb, 5 µm, 100 x 4.6 mmPart Number: 35005-104630Mobile Phase: 0.1% NH3 (aq)+ 0.1% DEAFlow Rate: 1 mL/minDetection: ELSD (120 °C, 3.5 L/min N2)

1. Hydrazine

HydrazineH350-1048

Column: Hypersil GOLD™, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: 20 mM NH4COOH at pH 3.0


1. Methylene Blue2. Methylene Red

DyesH250-094

1



Part Number: 73405-307746Mobile Phase: H2OFlow Rate: 1 mL/minDetection: ELSD

Polyethylene glycols and oxides

Polyethylene Glycolsand Oxides

K734-002

0 2 4 6 8 10 MIN

1

2

3

4

5

Column: Hypercarb™, 5 µm, 100 x 4.6 mmPart Number: 35005-104630Mobile Phase: A: ACN + 0.1%TFA

B: THF + 0.1%TFAGradient: 0 to 100 % B in 15 minFlow Rate: 1 mL/minDetection: UV at 254 nmTemperature: 22 °C1. Diethyl phthalate 3. Di-n-butyl-phthalate2. Dimethyl phthalate 4. Di-n-octyl phthalate

Phthalate EstersH350-1098


B: Phosphate buffer 10 mM at pH 2Isocratic: 35:65Flow Rate: 1 mL/minDetection: UV at 254 nmTemperature: 25 °CSource: Wan, Shaw, Davies and Barrett,

Nottingham University, UK

1. m-Aminobenzoic acid2. p-Aminobenzoic acid3. o-Aminobenzoic acid

AminobenzoicAcid Isomers

H350-1055

0 5 10 15MIN

Column: Hypercarb, 7 µm, 100 x 4.6 mmPart Number: 35007-104646Mobile Phase: H2OFlow Rate: 1 mL/minDetection: UV at 254 nmTemperature: 180 °CSource: R. M.Smith and R. J. Burgess,

University Loughborough, UK

1. Aniline2. N-Methylaniline3. N-Ethylaniline

Anilines (UHT-LC)H350-1113


B: ACNIsocratic: 80:20Flow Rate: 1 mL/minDetection: UV at 254 nm

1. Uracil 3. Resorcinol2. Phloroglucinol 4. Phenol

PhenolsH350-1046

Industrial

Applications


Pyrolysis of HighDensity PolyethyleneColumn: TR-1, 30 m x 0.32 mm x 0.5 µmPart Number: 260A224PTemperature: 50 °C, 10 °C/min to 320 °C and

hold for 10 minDetector Type: FIDCarrier Gas: H2

1. Polyethylene

20073b

TerpenesColumn: TR-35MS, 30 m x 0.25 mm

x 0.25 µmPart Number: 260C142PInitial Temp: 40 °C, 0.5 minRate 1: 10 °C/min to 200 °CFinal Temp: 200 °C, 1 minDetector Type: MSDetection TRACE DSQ MS, source 225 °C, Conditions: 35-500 m/z, EI @ 70 eVCarrier Gas: HeFlow Rate: 1 mL/minInjection Temp: 200 °CInjection Mode: SplitSplit Ratio: 50:1

1. α-pinene 10. dl-menthol2. Camphene 11. Borneol3. β-pinene 12. l-α-terpineol4. d-limonene 13. Dihydrocarveol5. p-cymene 14. Citronellol6. α-terpinene 15. Geraniol7. Linalool 16. Pulegone8. Fenchone 17. 2-piperidone9. l-isopulegol

11040501

PhenonesColumn: Hypersil GOLD™, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: 0.1% Formic acid


1. Uracil2. Acetophenone3. Propiophenone4. Butyrophenone5. Valerophenone6. Hexanophenone7. Heptanophenone8. Octanophenone

H250-023


UltraFast Determinationof VOCs in PackagingMaterials by Headspace GCColumn: TR-1701, 10 m x 0.1 mm x 0.1 µmPart Number: UFMC00400000000Temperature: 35 °C, then 1.5 °C to 200 °CDetector Type: FIDCarrier Gas: HeFlow Rate: 1.2 mL/minInjection Mode: SplitSplit Ratio: 250:1

1. Ethanol2. Acetone3. Ethyl Acetate4. Methylethyl ketone5. Toluene

AN10132

Grob TestColumn: TR-WaxMS, 30 m x 0.25 mm x

0.25 µmPart Number: 260X142PTemperature: 40 °C 1 min, 6 °C/min to 160 °C,

hold 5 minDetector Type: MSCarrrier Gas: He 25.7 psi, 35cm/sFlow Rate: 1.8 mL/minInjection 1 µLVolume:Injection Mode: Split 50:1, 250 °C

1. n-Decane 7. Dicyclohexylamine2. n-Undecane 8. Methyl undecanoate3. 1-Nonanal 9. Methyl dodecanoate4. 2,3-Butanediol 10. 2,6-Dimethylaniline5. 1-Octanol 11. 2,6-Dimethylphenol6. Methyl decanoate 12. 2-Ethylhexanoic acid

260X010


Industrial

Applications


Megamix of SemivolatilesColumn: TR-35MS, 30 m x 0.25 mm

x 0.25 µmPart Number: 260C142PTemperature: 40 °C, 1 min, 15 °C/min to 320 °C,

hold 12 minDetector Type: MSDetection TRACE DSQ MS, source 225 °C, Conditions: 50-650 m/z, EI @ 70 eVCarrier Gas: HeFlow Rate: 1 mL/minInjection Temp: 250 °CInjection Mode: PTV splitSplit Ratio: 1:20

06040502

1. Pyridine2. n-nitrosodimethylamine3. phenol4. 2-chlorophenol5. bis(2-chloroethyl)ether6. 1,3-dichlorobenzene7. Aniline8. 1,4-dichlorobenzene9. bis(2-chloroisopropyl)ether10. 1,2-dichlorobenzene11. o-cresol12. Hexachloroethane13. Benzylalcohol14. p-cresol15. m-cresol16. Nitrobenzene17. Isophorone18. 2,4-dimethylphenol19. 2-nitrophenol20. Hexachloro-1,3

-butadiene21. 2,4-dichlorophenol22. 1,2,4-trichlorobenzene23. Naphthalene24. 4-chloroaniline25. Hexachloro-cyclopentadiene26. 4-chloro-3-methylphenol27. 2-methylnaphthalene28. 1-methylnaphthalene29. 2,4,6-trichlorophenol30. 2,4,5-trichlorophenol31. 2-chloronaphthalene32. Dimethylphthalate33. 2-nitroaniline34. Acenaphthylene35. Acenaphthene36. 2,6-dinitrotoluene37. 1,4-dinitrobenzene

38. Dibenzofuran39. 1,2-nitrobenzene40. 2,3,4,6 - tetrachlorophenol41. 2,3,5,6-tetrachlorophenol42. 3-nitroaniline43. 2,4-dinitrophenol44. 4-nitrophenol45. Diethylphthalate46. 4-chlorophenyl

phenyl ether47. Fluorene48. Azobenzene49. Diphenylamine50. 4,6-dinitro-2-methylphenol51. Hexachlorobenzene52. 4-bromophenyl

phenyl ether53. 4-nitroaniline54. Pentachlorophenol55. Phenanthrene56. Anthracene57. Di-n-butylphthalate58. Carbazole59. Fluoranthene60. bis(2-ethylhexyl)

phthalate61. Pyrene62. Benzylbutyl phthalate63. bis(2-ethylhexyl)

phthalate64. Benz(a)anthracene65. Chrysene66. Di-n-ocylphthalate67. Benzo(b)fluoranthene68. Benzo(k)fluoranthene69. Benzo(a)pyrene70. Dibenz(a,h)anthracene71. Benzo(g,h,i)perylene


Hydrocarbon StandardColumn: TR-SimDist, 10 m x 0.53 mm

x 0.9 µmPart Number: 260F250PTemperature: 40 °C, 10 °C/min to 39 0 °C,

hold 10 minDetector Type: FIDDetection 400 °CConditions:Carrier Gas: HeFlow Rate: 20 mL/min

Hydrocarbon Standard Mix

24060510

Non-Ionic SurfactantsColumn: Hypercarb, 7 µm, 100 x 4.6 mmPart Number: 35007-104630Mobile Phase: A: H2O

B: ACNC: CH2Cl2

Gradient: Time (min) % A % B % C0 80 20 0

15 0 100 040 0 20 80

Flow Rate: 1 mL/minDetection: ELSDSource: P. Chaimbault, Journal of

Chromatography A, 797, 83-91 (1998)

PEG 400 and Triton X-100

H350-1053

0 10 20 30 40 MIN

PEG400 Triton X100 (PEAP)

Organic AcidsColumn: TR-WaxMS, 30 m x 0.25 mm x

0.25 µmPart Number: 260X142PTemperature: 70 °C 1 min, 10 °C/min to 180 °C

and hold 5 minDetector Type: MSCarrrier Gas: He 8.8 psiFlow Rate: 1 mL/minInjection 0.1 µLVolume:Injection Mode: Split 100:1, 250 °C

260X012

1. Pentanoic acid2. Hexanoic acid3. Heptanoic acid

4. Octanoic acid5. Nonanoic acid


Industrial

Applications


Halogenated CompoundsColumn: TR-5MS, 30 m x 0.25 mm x 1 µmPart Number: 260F296PTemperature: 40 °C 3 min, 8 °C/min to 90 °C,

6 °C/min to 200 °C, hold 5 minDetector Type: MSCarrrier Gas: HeFlow Rate: 1.8 mL/minInjection 1 µLVolume:Injection Mode: Split 250 °C 40:1

260F013

1. Chloromethane2. Vinyl chloride3. Chloroethane4. Chloroethane5. Trichlorofluoromethane6. 1,1-Dichloroethene7. Dichloromethane8. trans-1,2-Dichloroethene 9. 1,1,-Dichloroethane10. Unknown11. Chloroform12. 1,1,1-Trichloroethane13. Carbon tetrachloride14. Benzene15. 1,2-Dichloroethane16. Trichloroethene

17. 1,2-Dichloropropane18. 2-Chloroethylvinyl ether19. Bromodichloromethane20. 1,3-Dichloropropene (Z)21. Toluene22. 1,3-Dichloropropene (E)23. 1,1,2-Trichloroethane24. Tetrachloroethene25. Dibromochloromethane26. Chlorobenzene27. Ethylbenzene28. Bromoform29. 1,1,2,2-Tetrachloroethane30. 1,3-Dichlorobenzene31. 1,4-Dichlorobenzene32. 1,2-Dichlorobenzene

Tasmanian Lavander OilColumn: TR-WaxMS, 30 m x 0.25 mm x


220 °C 5 minDetector Type: MSCarrrier Gas: HeFlow Rate: 1.8 mL/minInjection 0.2 µLVolume:Injection Mode: Split 100:1, 250 °C

1. 3-Octanone 7. Linalyl acetate2. Octenyl acetate 8. Terpinen-4-ol3. Octanol 9. Lavandulyl acetate4. cis-Linalool oxide 10. L-Borneol5. trans-Linalool Oxide 11. Caryophyllene oxide6. L-Linalool

260X011

Analysis of Lighter FuelColumn: TR-5MS, 60 m x 0.32 mm x 1 µmPart Number: 260F155PTemperature: 30 °C isothermal 5 minDetector Type: FIDDetection: 270 °CCarrrier Gas: He, 1.94 psiFlow Rate: 1.7 mL/minInjection 10 µLVolume:Injection Mode: 250 °C, split 100:1

1. Propane2. i-butane3. Butane

260F011


Analysis of GasolineColumn: TR-5MS, 30 m x 0.25 mm x 0.25 µmPart Number: 260F142PTemperature: -20 °C for 1 min, 4 °C/min to

40 °C, 8 °C/min to 150 °CDetector Type: FIDCarrrier Gas: H2, 10 psiInjection Mode: Split

260F012

1. i-butane2. n-butane3. i-pentane4. n-pentane5. 2,2-dimethylbutane6. 2,3-dimethylbutane7. 2-methylpentane8. 3-methylpentane9. n-hexane10. benzene11. 2-methylhexane12. 2,3-dimethylpentane13. 3-methylhexane14. 2,2,4-trimethylpentane15. n-heptane16. toluene

17. 2,3-dimethylhexane18. ethylbenzene19. m-xylene20. p-xylene21. o-xylene22. n-propylbenzene23. 1-methly-3-ethylbenzene24. 1-methyl-4-ethylbenzene25. 1,3,5-trimethylbenzene26. 1-methyl-2-ethylbenzene27. 1,2,4-trimethylbenzene28. 1,2,3-trimethylbenzene29. naphthalene30. 2-methylnaphthalene31. 1-methylnaphthalene

Industrial SolventsColumn: TR-WaxMS, 30 m x 0.32 mm x

0.5 µmPart Number: 260X224PTemperature: 35 °C 3 min, 15 °C/min to

230 °C, hold 4 minDetector Type: FIDDetection: 270 °CCarrrier Gas: He 8.4 psi, 30cm/sFlow Rate: 1.84 mL/minInjection Volume: 0.1 µLInjection Mode: Split 83:1, purge on vent

150 mL/min

260X013

1. Acetone2. Ethyl acetate3. Methyl ethyl ketone4. Contaminant5. iso-Propanol6. Ethanol7. Methyl isobutyl

ketone8. Toluene

9. Butyl acetate10. iso-Butanol11. Propylene glycol

Monomethyl ether12. n-Butanol13. Ethyl benzene14. p-Xylene15. m-Xylene16. o-Xylene

17. Butyl Cellosolveacetate

18. Cyclohexanone19. Butyl Cellosolve20. Butyl glycol

acetate22. Isophorone23. Butyl Carbitol24. Benzyl alcohol

Triton™ X-100 (UHT-LC)Column: Hypercarb™, 5 µm, 100 x 1 mmPart Number: 35005-101046Mobile Phase: A: ACN

B: CH2Cl2Gradient: 30 to 100% B in 3.5 minFlow Rate: 0.2 mL/minDetection: MS Temperature: 140 °CSource: Sabine Heinische, Laboratoire of

Sciences Analytiques, Universite Lyon, France

Triton X-100

H350-1122

Industrial

Applications


21040501

PolysulphidesColumn: Hypercarb™, 7 µm, 100 x 4.6 mmPart Number: 35007-104630Mobile Phase: Panel A: Butyl

Chloride/Isopentane (40:60)Panel B: ButylChloride/Isopentane (5:95)

Flow Rate: 0.5 mL/minDetection: UV at 254 nmSource: Data Courtesy of Dr. Mockel,

Hahn-Meiter Institut, Berlin, Germany

1. (CH3)2 (H)2 Sx

7034

A B

Analysis of FragranceAllergensColumn: TR-WAX 30 m x 0.32 mm ID x

0.25 µmPart Number: 260W143PTemperature: 80 °C, hold 2 min, 10 °C/min to

120 °C, hold 4 min, 10 °C/min to155 °C, hold 4 min, 10 °C/min to250 °C, hold 3 min/ (Inlet: 250 °C)

Detector Type: DSQ™ MSCarrier Gas: HeFlow Rate: 1 mL/minInjection Volume: 1 mLInjection Mode: Split 100:1

260W013

1. Limonene2. Linalool3. Methyl 2-octynoate4. Citral (1)5. 1,4-Dobromobenzene (ISTD)6. Citral (2)7. Citronellol8. α-isomethyl ionone9. Geraniol10. Benzyl Alcohol11. Hydroxycitronellol12. Cinnamealdehyde13. Lilal14. Eugenol

15. Amylcinnamaldehyde16. Anise Alcohol17. Cinnamyl Alcohol18. Farnesol (1)19. Farnesol (2)20. Isoeugenol21. α –Hexyl cinnamaldehyde22. Farnesol (3)23. Coumarin24. Benzyl Benzoate25. Salicylic Acid26. 4,4'-Dibromobiphenyl (ISTD)27. Benzyl Cinnamate


Column: Hypercarb, 7 µm, 100 x 4.6 mmPart Number: 35007-104630Mobile Phase: ACNFlow Rate: 0.8 mL/minDetection: UV at 254 nm

1. o-Nitrotoluene2. m-Nitrotoluene3. p-Nitrotoluene

Nitrotoluenes7024

Column: Hypersil GOLD™, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: 0.1% Phosphoric acid

B: ACN:0.1% Phosphoric acid (95:5)Gradient: Time (min) %B

0 02 0

25 80Flow Rate: 1.25 mL/minDetection: UV at 270 nmTemperature: 25 °C

1. Pyridine 5. Phenol2. Benzylamine 6. 4-Nitrobenzoic Acid3. N-acetylprocainamide HCl 7. 2,3-Dihydroxynaphthalene4. Benzyl Alcohol 8. 4-Chlorocinnamic Acid

Acids, Bases and NeutralsH250-056



1. Phenol2. 4-Nitrophenol3. 2,6-Dimethylphenol4. 3,5-Dimethylphenol

PhenolsH250-062

Column: Hypercarb, 5 µm, 100 x 1.0 mmPart Number: 35005-101046Mobile Phase: H2O + 20 mM Formic acidFlow Rate: 0.1 mL/minDetection: FIDTemperature: 100 °C for 1.2 min; 100 to

180 °C in 2.6 minSource: S. Heinische, D. Guillarme,

Laboratoire des Sciences Analytiques, Univ. Lyon, France

1. Acetic acid 3. Butyric acid2. Propionic acid 4. Cyclohexane carboxylic acid

Carboxylic Acids (UHT-LC)H350-1112

Column: Hypercarb, 5 µm, 100 x 1 mmPart Number: 35005-101046Mobile Phase: H2OFlow Rate: 0.1 mL/minDetection: FID Temperature: 100 °CSource: Sabine Heinische, Laboratoire des

Sciences Analytiques, Université Lyon, France

1. Methanol 4. Butanol2. 2-Propanol 5. Methyl-2-butanol3. 1,2-Butanediol 6. Pentanol

Alcohols (UHT-LC)H350-1109

Column: Hypercarb™, 5 µm, 100 x 4.6 mmPart Number: 35005-104630Mobile Phase: A: 10 mM 1-methylpiperidine

at pH 10.5B: ACN/IPA (1:1)

Gradient: 50 to 90% B in 10 minFlow Rate: 1 mL/minDetection: UV at 270 nmTemperature: 25 °C

1. Aniline 4. N-ethylaniline2. 3-ethylaniline 5. N,N-dimethylaniline3. 2-ethylaniline 6. N,N-diethylaniline

AnilinesH350-1060

Industrial

Applications


Acrylamide in Cooked FoodThe excellent retention, peak shape and reproducibility of Hypercarb columnsallows accurate measurement of acrylamide in a wide variety of foods.

In April 2002, a research group at the Swedish National FoodAdministration published a paper in The Analyst demonstrating thepresence of acrylamide at elevated levels in cooked food.1 Acrylamideis a suspected carcinogen and although no link has been provenbetween acrylamide and cancer in humans, the World HealthOrganization has described its presence in food as “a major concern”.

Acrylamide is formed naturally in foods with high starch contentduring cooking, with elevated concentrations of acrylamide detectedin french fries, potato chips, breads and processed cereals, particularlyafter cooking using a microwave. Consequently, several food agenciesand proficiency testing schemes are recommending more research todetermine ways to minimize its concentration in food. These findingsattracted worldwide attention, increasing demand for fast, sensitiveanalytical methods.

Traditional methods of analysis for acrylamide involve samplederivatization followed by gas chromatography. This application notereports a simple and accurate method for the analysis of acrylamidein cooked food using the polar retention capacity of Hypercarbcolumns for a faster LC/MS technique.

Acrylamide has a high degree of polarity and shows limited capacity to interact with silica-based hydrophobic (C18) bonded phases.Such silica based columns show poor quantitation at the picogramlevel, as acrylamide elutes with the column void volume and is difficult to distinguish from other polar sample constituents.

Hypercarb (100% porous graphitic carbon) has a polarizable surfacethat is able to form charge induced dipole interactions with polar molecules which have a permanent dipole. This dipole-dipole interactionresults in strong retention of polar analytes, which are not retainedon silica-based phases. This capability to create charge induced interactions gives Hypercarb far greater retention for polar compoundsthan silica-based phases.


Column: Hypercarb™ 5 µm 50 x 2.1 mmPart Number: 35005-052130Mobile Phase: H2OGradient: IsocraticInjection Volume: 10 µLFlow Rate: 0.4 mL/minDetection: + ESI SIM ([M + H]+, m/z = 72)

Results and DiscussionThis method gives a retention time of 1.8 minutes for acrylamide with k' = 3.6, which gives adequate retention beyond the column voidvolume for accurate quantification (Figure 1a). This is highlighted bythe linearity of response for the method over a concentration range 1 to 1000 ng/mL, as shown in Figure 1b.

References1. J. Rosèn & K-E. Hellenäs The Analyst, 2002 127 pp 880–882

Figure 1: Retention of acrylamide on Hypercarb and linearity range. The method gives a linear response enabling accurate quantitation.

(a)

(b)

221002_01

Analysis of Water-Soluble Vitamins on a Polar Endcapped C18Stationary PhaseWater-soluble vitamins are retained and resolved using a Hypersil GOLD aQ column andmobile phase conditions which are ideal for sensitive detection using positive ESI.

Vitamins are a group of chemically unrelated compounds which occur in small amounts in biological materials. Because of their nutritional importance, it is necessary to have sensitive and robustanalytical methods to determine vitamins in food materials anddietary supplements.

HPLC is commonly used for the determination of vitamins, butthe analysis of water-soluble vitamins by reversed phase HPLC(RP–LC) can be challenging since these compounds have very differ-ent chemical structures and therefore exhibit different retentionbehaviors. The smaller, more polar vitamins such as thiamine showlittle retention in RP–LC, whereas the more hydrophobic vitaminssuch as riboflavin are well retained. Gradient conditions are neces-sary to elute all analytes within a reasonable analysis time.Moreover, polar vitamins are difficult to retain on typical reversedphase columns unless high concentrations of non-volatile buffers oreven ion pairing reagents are used. These mobile phase conditionsare not amenable to high sensitivity LC/MS methods.

The use of a polar endcapped C18 phase has the advantage ofretaining the polar water-soluble vitamins sufficiently to allow foraccurate quantification, even when acidic, volatile mobile phase addi-tives are used. The polar functional group used to endcap HypersilGOLD aQ media provides an interaction mechanism in addition to thedispersive interaction with the alkyl chain, by which polar compoundscan be retained and resolved. Additionally, because this phase is builtupon the technology of Hypersil GOLD™ silica, symmetrical and efficientpeaks are obtained even with weakly buffered mobile phases.


Column: Hypersil GOLD aQ™, 5 µm, 150 x 4.6 mmPart Number: 25305-154630Mobile Phase: A: H2O + 0.1% Formic acid

B: ACN + 0.1% Formic acidGradient: 4% B for 3 min then to 100% B by 12 minFlow Rate: 1.0 mL/minDetection: UV at 266 nmTemperature: 25 °C

Results and DiscussionThe six water-soluble vitamins are retained and separated on aHypersil GOLD aQ column using a gradient of water and acetonitrilewith 0.1% formic acid, conditions which promote good ionization forsensitive detection in positive electrospray. Analysis is completed inless than 8 minutes and the peak shape is very symmetrical for allanalytes. Transfer of this method to LC/MS will only require reductionof the column internal diameter to 2.1 mm and reduction of flow rateto 0.2 mL/min.

Figure 1: The analysis of water-soluble vitamins on a polar endcapped C18phase illustrates the enhanced retention of polar compounds using HypersilGOLD aQ columns.

1. Thiamine monophosphate; 2. Thiamine; 3. Unknown; 4. Pyridoxal; 5. Pyridoxal-5-phosphate; 6. Pyridoxine; 7. Unknown; 8. Riboflavin

H253-005


Food Safety

Applications


Selectivity Screening in the HPLC Analysis of CatechinsThe selectivity changes that can be obtained with alkyl chain, cyano and perfluorinatedchemistries when using generic mobile phases are illustrated for a mixture of catechins. Thisapproach for stationary phase screening can significantly reduce method development time.

In traditional Chinese medicine, green tea has been used as an astrin-gent, cardiotonic, central nervous stimulant and a diuretic. Most ofthe healthful properties of green tea are attributed to the catechins,which are polyphenols with a flavonoid structure. The selectivity ofthree column chemistries for the high performance liquid chromatog-raphy (HPLC) separation of a mixture of catechins was evaluated.

Following the success of the Hypersil GOLD stationary phase forproviding extremely symmetrical peaks, even for very basic analytes,additional chemistries have been developed using the same highlypure silica support and robust bonding process. These include cyanoand perfluorinated chemistries. Hypersil GOLD CN offers a cyanochemistry with alternative selectivity for reversed phase and can alsobe used for normal phase separations. Hypersil GOLD PFP has apentafluorophenyl ligand that provides extra selectivity for halogenatedcompounds. It also performs well for molecules which contain severalnitro, hydroxyl, carboxyl or other polar groups and that may not bewell retained or resolved on alkyl chain phases. The introduction of afluorine group in the stationary phase causes significant changes inthe solute-stationary phase interactions. The carbon-fluorine bond ismore polar than the carbon-hydrogen bond, which explains the extraselectivity and retention observed for compounds containing halogensand polar functional groups.


Columns: Hypersil GOLD™ 5 µm, 150 x 4.6 mmHypersil GOLD PFP 5 µm, 150 x 4.6 mmHypersil GOLD CN 5 µm, 150 x 4.6 mm

Part Numbers: 25005-15463025405-15463025805-154630

Mobile Phase: A: H2O + 0.1% Formic acid B: ACN + 0.1% Formic acid

Gradient: 20 to 50% B in 15 min Flow Rate: 1 mL/minDetection: UV at 280 nmTemperature: 25 °C

Results and DiscussionThe series of chromatograms shows the effect of changing the columnchemistry on the separation of catechins when a generic mobilephase is used. The Hypersil GOLD PFP produces a change in elutionorder of analytes 2 and 3, compared with the alkyl chain phase. Theextra retention of epigallocatechin gallate over epicatechin is thoughtto be caused by the additional substituted ring, which interacts withthe phenyl ring on the perfluorinated stationary phase.

Similarly, these analytes also switch elution order on theHypersil GOLD CN column. This column also shows another reversalof elution order between gallocatechin gallate and epicatechin gallate.This is likely to be caused by the additional hydroxy group in gallocat-

echin gallate. Screening different column chemistries with a genericmobile phase can significantly reduce method development time inreverse phase HPLC.

Figure 1: Separation of catechins on three column chemistries: C18 selectivity,perfluorinated phenyl, and cyano.

1. Catechin

2. Epigallocatechin gallate

6. Catechin gallate

5. Epicatechin gallate

4. Gallocatechin gallate

3. Epicatechin

Analytes:

Food Safety

Water Soluble Vitaminsfrom Aqueous SolutionsCompounds: Niacinamide, pyridoxine, riboflavin,

thiaminePart Number: 60108-304Phase: HyperSep C18Volume: 3 mLBed Weight: 500 mgSample Use an amber glass bottle. Pretreatment: Mix 50 mL sample with riboflavin

content < 6 mg with 0.5 mL aceticacid and 0.1 g heptane-1-sulphonicacid sodium salt. Flush bottle withnitrogen, heat to 55 °C, shake.Cool down rapidly.

Conditioning: 3 mL Methanol followed by 3 mLof a solution of 0.5 mL acetic acidand 0.1 g heptane-1-sulfonic acidsodium salt in 50 mL water (to beprepared daily)

Application: 2 mL sample solution to be forced or aspirated through column

Washing: 2 x 250 µL of a solution of 0.5 mLacetic acid and 0.1 g heptane-1-sulphonic acid sodium salt in 50 mL water

Elution: 3 x 500 µL methanol – Immediate analysis required

Aflatoxin M1 Mycotoxinfrom MilkCompounds: Aflatoxin M1Part Number: 60108-305Phase: HyperSep™ C18Volume: 6 mLBed Weight: 500 mgSample Dilute 20 mL milk with 30 mLPretreatment: distilled waterConditioning: 10 mL methanol followed by

10 mL distilled waterApplication: Force or aspirate sample slowly

through columnWashing: 10 mL distilled water followed by

10 mL n-hexane – then dry column at 50 °C for 10-20 min or at ambient temp overnight

Elution: 3 mL dichloromethane/acetone (4:1, v/v)

Anthocyan Dyes fromRed WineCompounds: Anthrocyan dyePart Number: 60108-309Phase: HyperSep C8Volume: 3 mLBed Weight: 500 mgConditioning: 3 mL methanol followed by 3 mL

distilled waterApplication: Force or aspirate wine sample

slowly through columnWashing: 1.5 mL distilled waterElution: Small volume methanolic HCl

Folic Acid from FoodCompounds: Folic acidPart Number: 60108-521Phase: HyperSep SAXVolume: 3 mLBed Weight: 500 mgSample Homogenize 10 g food sample Pretreatment: in 100 mL 0.01 M phosphate buffer

pH 7.4. FilterConditioning: 6 mL n-hexane followed by 6 mL

methanol and 6 mL distilled waterApplication: Force or aspirate 10 mL filtrate

through columnWashing: 6 mL distilled waterElution: 5 mL 10% NaCl in 0.1 M sodium

acetate buffer

Column: HyperREZ™ XP Carbohydrate Ca2+, 8 µm, 300 x 7.7 mm

Part Number: 69208-307780Mobile Phase: H2OFlow Rate: 0.6 mL/minDetection: ELSTemperature: 85 °C

1. Sucrose2. Glucose3. Fructose

Fruit JuicesHR2001

Column: Hypersil GOLD™ CN, 5 µm, 150 x 4.6 mm

Part Number: 25805-154630Mobile Phase: A: 25 mM KH2PO4 pH 2


1. 4-Fluorobenzoic Acid 4. 2,4,6-Trimethylbenzoic Acid2. o-Toluic Acid 5. 2,5-Dimethylbenzoic Acid3. p-Toluic Acid

Organic AcidsH258-002


Food Safety


Applications


Column: Hypersil GOLD™, 1.9 µm, 20 x 2.1 mmPart Number: 25002-022130Mobile Phase: A: 0.1% Formic acid

B: ACN + 0.1% Formic acidIsocratic: 12:88Flow Rate: 0.1 mL/minDetection: +ESITemperature: 25 °C

1. Impurity from Sudan II 4. Sudan II2. Impurity from Sudan IV 5. Sudan III3. Sudan I 6. Sudan IV

Sudan DyesH250-086

Column: BioBasic AX, 5 µm, 150 x 4.6 mmPart Number: 73105-154630Mobile Phase: A: ACN

B: H2O Isocratic: 75:25Flow Rate: 1 mL/minDetection: ELS

1. Glucose2. Maltose3. Maltotriose4. Maltotetraose5. Maltopentaose

Sugars in HILIC ModeK731-003

Column: BioBasic™ SCX, 5 µm, 150 x 4.6 mmPart Number: 73205-154630Mobile Phase: A: 50 mM KH2PO4 at pH 3

B: 0.5 M KH2PO4 at pH 3Gradient: Time (min) % B

0 106 106.1 100

Flow Rate: 1 mL/minDetection: UV at 254 nmTemperature: 50 °C

1. Vitamin B122. Vitamin B23. Vitamin B64. Vitamin B1

VitaminsK732-007


Part Number: 73505-307746Mobile Phase: H2OFlow Rate: 1 mL/minDetection: ELSD

1. Pullulan 8002. Pullulan 503. Pullulan 54. Sucrose

PullulansK735-001

0 2 4 6 8 10 12 14 16 18 MIN

12

3

4

Column: HyperREZ™ XP Carbohydrate H+, 8 µm, 300 x 7.7 mm

Part Number: 69008-307780Mobile Phase: 5 mM H2SO4


1. Anthocyanins2. Tartaric acid3. Malic acid4. Succinic acid5. Acetic acid

Organic Acids in Wine9020

Column: HyperREZ XP Carbohydrate Na+,10 µm, 300 x 7.8 mm

Part Number: 69310-307780Mobile Phase: H2OFlow Rate: 0.3 mL/minDetection: RITemperature: 80 °C

1. Dp1 6. Dp62. Dp2 7. Dp73. Dp3 8. Dp84. Dp4 9. Dp95. Dp5

Corn Syrup9024


Column: HyperREZ™ XP Carbohydrate Pb2+, 8 µm, 300 x 7.7 mm

Part Number: 69108-307780Mobile Phase: H2OFlow Rate: 0.6 mL/minDetection: RITemperature: 80 °C

1. Polysaccharides 2. Maltose3. Ethanol4. Glycerol

Alcohol Levels in Beer9021

Column: HyperREZ XP Sugar Alcohols, 8 µm, 250 x 4.0 mm


B: ACN Isocratic: 70:30Flow Rate: 0.3 mL/minDetection: RITemperature: 60 °C

1. Pentaerythritol 5. Mannitol2. Erythritol 6. Xylitol3. Adonitol 7. Dulcitol4. Arabitol 8. Sorbitol

Sugar Alcohols9026

1

1

2

3

45

67

8

0 10 MIN

Column: Hypercarb™, 5 µm, 100 x 3.0 mmPart Number: 35005-103030Mobile Phase: A: Dioxane

B: CHCl3Isocratic: 10:90Flow Rate: 0.8 mL/minDetection: Fluorescence

(exc 365 nm, em 418 nm)Source: Rhemrev-Boom,

M.M, Amro Emmen

1. Aflatoxin B1

2. Aflatoxin B2

3. Aflatoxin G1

4. Aflatoxin G2

afla1

Aflatoxins

43

2

1

Column: Hypersil GOLD5 µm, 150 x 4.6 mm

Part Number: 25005-154630Mobile Phase: A: ACN


1. Vitamin A2. Vitamin D23. Vitamin D34. Vitamin E5. Vitamin E Acetate6. Vitamin K1

Fat Soluble VitaminsH250-055

Column: Hypercarb, 5 µm, 50 x 2.1 mmPart Number: 35005-052130Mobile Phase: H2OFlow Rate: 0.4 mL/minDetection: +ESITemperature: Ambient

1. Acrylamide

Acrylamide in Foodstuffs221002_01

Column: Hypersil GOLD™ C8, 5 µm, 150 x 4.6 mm



1. Linolenic Acid2. Linoleic Acid

Linoleic AcidH252-004

Food Safety

Applications


Column: Hypercarb, 7 µm, 100 x 4.6 mmPart Number: 35007-104630Mobile Phase: A: 10% ACN in 20 mM EDTA

B: 50% ACN in 20 mM EDTAGradient: 0 to 100% B in 40 minFlow Rate: 1 mL/minDetection: UV at 276 nmSource: J. N. Done, United Distillers, UK

1. Maltol2. Ethyl Maltol3. Vanillin

Flavors in a Beverage7003

Column: Hypercarb, 3 µm, 100 x 2.1 mmPart Number: 35003-102130Mobile Phase: A: 0.1% NH3 (aq) at pH 10.3

B: ACNIsocratic: 96:4Flow Rate: 0.2 mL/minDetection: - ESITemperature: 60 °C

1. Sucrose2. Maltose3. Lactose

Disaccharides24090301

Column: Hypercarb™, 7 µm, 100 x 4.6 mmPart Number: 35007-104630Mobile Phase: A: 0.025 mM Sorbic acid

+ 0.1 M NaOHB: MeOH

Isocratic: 90:10Flow Rate: 1 mL/minDetection: Indirect UVTemperature: 22 °CSource: Steffanson, Uppsala

University, Sweden

1. Melibiose2. Sucrose3. Lactose4. System peak (sorbic acid) 5. Melizitose6. Gentiobiose7. Cellobiose

Di- and Tri-SaccharidesH350-1083

CarbohydratesColumn: Hypercarb, 5 µm, 100 x 4.0 mmPart Number: 35005-104030Mobile Phase: A: ACN

B: NH3 (aq) at pH 11 Isocratic: 4:96 (v/v)Flow Rate: 1 mL/minDetection: ELSDTemperature: 60 °C

1. Isomaltose2. Melibiose3. Maltose4. Lactose5. Cellobiose

11080301

1

2

3

4

5


Column: Hypercarb, 7 µm, 100 x 4.6 mmPart Number: 35007-104630Mobile Phase: 300 mM Formic acid (aq)Flow Rate: 1 mL/minDetection: ELSDTemperature: 40 °CSource: C. Elfakir, P. Chaimbault, and M.

Dreux, Journal of ChromatographyA, 829 (1998) 193-199.

1. Cations 2. Hydrogen phosphate3. Sulphate4. Nitrate5. Perclorate

Inorganic IonsH350-1099

Oxygen HeterocyclesColumn: Hypercarb™, 7 µm, 100 x 4.6 mmPart Number: 35007-104630Mobile Phase: A: HClO4 (aq) at pH 1.0

B: ACNGradient: 1 to 35% B in 10 minFlow Rate: 1 mL/minDetection: UV at 280 nmSource: Data courtesy of Dr. A. Lea and

Dr. G. Ford, Reading ScientificServices Ltd, Reading, UK

1. DHHM2. Furaneol3. Cyclotene4. HMF5. HMP6. Maltol

7035

Column: Hypercarb, 5 µm, 100 x 4.6 mm (CTA 0.5 mM)

Part Number: 35005-104630Mobile Phase: 2 mM Na2CO3 + 1 mM NaHCO3 +

2.5% ACNFlow Rate: 1.2 mL/minDetection: Suppressed Conductivity

1. Fluoride2. Chloride3. Bromide4. Nitrate5. Phosphate6. Sulphate

AnionsH350-1032

Column: Hypercarb, 5 µm, 100 x 1.0 mmPart Number: 35005-101030Mobile Phase: H2OFlow Rate: 0.05 mL/minDetection: FIDTemperature: 25 °CSource: Sabine Heinische, Laboratoire des

Sciences Analytiques, Université Lyon, France

1. Maltose2. Ribose3. Lyxose4. Sorbose

SugarsH350-1082

1

2

3

4

5

Food Safety

Applications



Part Number: 25405-154630Mobile Phase: A: H2O + 0.1% Formic acid


1. Vitamin C (ascorbic acid)2. Uracil

Vitamin CH254-001


Part Number: 25205-154630Mobile Phase: MeOHFlow Rate: 1.5 mL/minDetection: UV at 450 nmTemperature: 25 °C

1. Lutein2. Lycopene3. β-Carotene

β-CaroteneH252-009

Energy Drink AdditivesColumn: Hypersil GOLD™, 5 µm,

150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: 10 mM NH4OAc at pH 5.0

B: MeOH Gradient: 30 to 45% B in 10 minFlow Rate: 1 mL/minDetection: UV at 230 nmTemperature: 25 °C

1. Acesulfame2. Saccharin3. Caffeine4. Benzoic acid5. Sorbic acid6. Aspartame

H250-009

Column: Hypersil GOLD aQ™


B: ACN + 0.1% Formic acidGradient: 4% B for 3 min, then to 100% B

by 12 minFlow Rate: 1.0 mL/minDetection: UV at 266 nmTemperature: 25 °C

1. Thiamine monophosphate2. Thiamine3. Unknown4. Pyridoxal5. Pyridoxal-5-phosphate6. Pyridoxine7. Unknown8. Riboflavin

Water Soluble VitaminsH253-005


Methylamines in FishColumn: Hypercarb™, 7 µm, 100 x 4.6 mmPart Number: 35007-104630Mobile Phase: 5 mM Heptanesulfonic acid +

5 mM KH2PO4 at pH 9Flow Rate: 1 mL/minSource: Lofti I. Monser, Analytica Chemica

Acta, 322 (1996) 63-68.

1. Trimethylamine (TMA)2. Dimethylamine (DMA)3. Methylamine (MA)

H350-1093

Column: Hypercarb, 7 µm, 100 x 4.6 mmPart Number: 35007-104630Mobile Phase: A: CH3COOH (aq)

B: ACN Gradient: 10 to 80% B in 40 minFlow Rate: 1 mL/minDetection: UV at 280 nmSource: J.N. Done, United Distillers,

UK (1988)

1. Phenol 7. 2-Ethylphenol2. Guaiacol 8. 3,5-Xylenol3. m-Cresol 9. 4-Ethyl guaiacol4. p-Cresol 10. Eugenol5. o-Cresol 11. Internal standard6. 4-Ethylphenol

Phenols in Whiskey7033

Column: Hypercarb, 5 µm, 100 x 4.6 mmPart Number: 35005-104630Mobile Phase: A: 50 mM NH4OAc at pH 6.0

B: ACN:IPA (1:1)C: THF

Gradient: Time (min) % B % C0 7 0

10 60 012 95 525 0 100

Flow Rate: 1 mL/minDetection: UV at 215 nm; 275 nm at 10 minTemperature: 25 °C

1. Vitamin B5 5. Vitamin B62. Vitamin B3 6. Vitamin A3. Vitamin H 7. Vitamin D34. Vitamin B12 8. Vitamin D2

Water and FatSoluble Vitamins

H350-1030

Column: Hypersil GOLD™, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: 20 mM NH4OAc at pH 4.1


1. Saccharin2. Caffeine3. Aspartame4. Benzoic acid5. Sorbic acid

Soft Drink AdditivesH250-007

Food Safety


Applications



B: MeOH + 0.1% Formic acidGradient: 5 to 100% B in 15 minFlow Rate: 0.3 mL/minDetection: - ESITemperature: 30 °C

1. Bilobalide2. Unknown (bilobalide)3. Ginkgolide C4. Unknown (ginkgolide C)5. Unknown (ginkgolide A)6. Ginkgolide A7. Ginkgolide B8. Unknown (ginkgolide A)9. Quercetin10. Kaempferol11. Unknown (kaempferol)

Ginkgo Biloba H250-017


B: ACN + 0.1% Formic acidGradient: 5 to 100% B in 15 minFlow Rate: 0.3 mL/minDetection: + ESITemperature: 30 °C

1. Capsaicin2. Related compound

CapsaicinH250-018

Column: Hypersil GOLD, 5 µm, 150 x 2.1 mmPart Number: 25005-152130Mobile Phase: A: H2O + 0.1% HFBA

(heptafluorobutyric acid)B: MeOH + 0.1% HFBA

Gradient: 30 to 100% B in 15 minFlow Rate: 0.2 mL/minDetection: + ESITemperature: 30 °C

1. Serotonin 6. Tryptamine2. Butylamine 7. Spermidine3. Cadaverine 8. Hexylamine4. Histamine 9. Spermine5. Phenylethylamine

Biogenic AminesH250-025


B: MeOHIsocratic: 5:95Flow Rate: 1 mL/minDetection: - ESITemperature: 30 °C

1. δ-Tocopherol2. γ-Tocopherol3. α-Tocopherol

TocopherolsH250-092



Part Number: 25005-154630Mobile Phase: A: 0.1% TFA


1. t0

2. Pentanoic acid3. trans-, trans-2-4-hexadienoic acid4. trans-2-hexenoic acid5. Hexanoic acid

Pentanoic and Hexanoic Acids

H250-091


Part Number: 25205-154630Mobile Phase: A: 0.05 M KH2PO4 pH 3.5

B: ACNGradient: 30 - 70% B in 15 minFlow Rate: 1.25 mL/minDetection: UV at 230 nmTemperature: 25 °C

1. Lidocaine2. Methyl Paraben3. Propyl Paraben

H252-002

Parabens



1. Methyl Paraben2. Ethyl Paraben3. Propyl Paraben4. Butyl Paraben

ParabensH250-082

Analysis of FAMEsColumn: TR-FAME, 30 m x 0.25 mm x

0.25 µmPart Number: 260M142PTemperature: 50 °C 2 min, then 4 °C/min to

250 °C, then hold 15 minDetector Type: MSCarrrier Gas: HeFlow Rate: 0.5 mL/minInjection 1 µLVolume:Injection Mode: Split 100:1

1. Butyric acid methyl ester (C4:0)2. Caproic acid methyl ester (C6:0)3. Caprylic acid methyl ester (C8:0)4. Capric acid methyl ester (C10:0)5. Undecanoic acid methyl ester (C11:0)6. Lauric acid methyl ester (C12:0)7. Tridecanoic acid methyl ester (C13:0)8. Myristic acid methyl ester (C14:0)9. Myristoleic acid methyl ester (C14:1)10. Pentadecanoic acid methyl ester (C15:0)11. cis-10-Pentadecenoic acid methyl ester (C15:1)12. Palmitic acid methyl ester (C16:0)13. Palmitoleic acid methyl ester (C16:1)14. Heptadecanoic acid methyl ester (C17:0)15. cis-10-Heptadecenoic acid methyl ester (C17:1)

16. Stearic acid methyl ester (C18:0)17. Oleic acid methyl ester (C18:1n9c)18. Elaidic acid methyl ester (C18:1n9t)19. Linoleic acid methyl ester (C18:2n6c)20. Linolelaidic acid methyl ester (C18:2n6t)21. g-Linolenic acid methyl ester (C18:3n6)22. Linolenic acid methyl ester (C18:3n3)23. Arachidic acid methyl ester (C20:0)24. cis-11-Eicosenoic acid methyl ester (C20:1)25. cis-11,14-Eicosadienoic acid methyl ester (C20:2)26. cis-8,11,14-Eicosatrienoic acid methyl ester (C20:3n6)

27. Heneicosanoic acid methyl ester (C21:0)28. cis-11,14,17-Eicosatrienoic acid methyl ester (C20:3n3)29. Arachidonic acid methyl ester (C20:4n6)30. cis-5,8,11,14,17-Eicosapentaenoic acid methyl ester (C20:5n3)31. Behenic acid methyl ester (C22:0)32. Erucic acid methyl ester (C22:1n9)33. cis-13,16-Docosadienoic acid methyl ester (C22:2)34. Tricosanoic acid methyl ester (C23:0)35. Lignoceric acid methyl ester (C24:0)36. cis-4,7,10,13,16,19-Docosohexaenoic acid methyl ester (C22:6n3)37. Nervonic acid methyl ester (C24:1)

Food Safety

Applications


Column: Hypersil GOLD, 5 µm, 150 x 4.6 mmPart Number: 25005-154630

A: 0.1% Formic acidB: ACN:0.1% Formic acid (95:5)

Gradient: 5 - 30% B in 20 minFlow Rate: 1.25 mL/minDetection: UV at 280 nmTemperature: 25 °C

1. 3,4-Dihydroxyphenyl Acetic Acid 6. Ferulic Acid2. p-Hydroxybenzoic Acid 7. m-Coumaric Acid3. Caffeic Acid 8. o-Coumaric Acid4. Vanillic Acid 9. Salicylic Acid5. p-Coumaric Acid

Organic AcidsH250-057

Column: Hypersil GOLD™, 5 µm, 150 x 4.6 mmPart Number: 25005-154630Mobile Phase: A: 0.1%Formic acid

B:ACNIsocratic: 70:30Flow Rate: 1 mL/minDetection: UV at 270 nmTemperature: 40 °C

1. Uracil 3. m-Coumaric Acid2. p-Coumaric Acid 4. o-Coumaric Acid

Coumaric AcidsH250-070



1. Gallic Acid 4. Caffeic Acid2. 3,4-Dihydroxphenyl Acetic Acid 5. m-Hydroxybenzoic Acid3. p-Hydroxybenzoic Acid

Aromatic Organic AcidsH250-071


CatechinsColumn: Hypersil GOLD aQ™


B: MeOH + 0.1% Formic acidGradient: 20 – 50%B in 15 minFlow: 1.0Detection: UV at 280 nmTemperature: 25 °C

1. Catechin 4. Gallocatechin Gallate2. Epigallocatechin Gallate 5. Epicatechin Gallate3. Epicatechin 6. Catechin Gallate

H253-002

Food Safety


24 FAMEsColumn: TR-FAME, 30 m x 0.25 mm

x 0.25 µmPart Number: 260M142PTemperature: 150 °C for 0.5 min, 10 °C/min to

180 °C, 1.5 °C/min to 220 °C, 30 °C/min to 260 °C, hold 5 min

Detector Type: FIDDetection 280°CConditions:Carrier Gas: He 20.7 psiFlow Rate: 1.3 mL/minInjection Volume: 1.0 µLInjection Details: Split 15:1, 250 °C

24060512

Rapeseed OilColumn: TR-WaxMS, 30 m x 0.25 mm x

0.25 µmPart Number: 260X142PTemperature: 195 °C 13 min, 20 °C/min to 220,

hold 5 min, 20 °C/min to 230 °C,hold 5 min

Detector Type: MSCarrrier Gas: He 39.2psiFlow Rate: 1.6 mL/minInjection 0.5 µLVolume:Injection Mode: Split 80:1, 250 °C

1. Methyl Myristate (C14:0)2. Methyl Palmitate (C16:0)3. Methyl Stearate (C18:0)4. Methyl Oleate (C18:1)5. Methyl Linoleate (C18:2)6. Methyl Linolenate (C18:3)7. Methyl Arachidate (C20:0)8. Methyl Eicosenoate (C20:1)9. Methyl Behenate (C22:0)10. Methyl Erucate (C22:1)11. Methyl Lignocerate (C24:0)

260X015

Nutmeg OilColumn: TR-WaxMS, 30 m x 0.25 mm

x 0.25 µmPart Number: 260X142PTemperature: 40 °C 1 min, 8 °C/min to 220 °C,

hold 5 minDetector Type: MSCarrrier Gas: He 25.7 psi, 35cm/sFlow Rate: 1.8 mL/minInjection 0.2 µLVolume:Injection Mode: Split 100:1, 250 °C

260X014

1. α-Pinene2. α-Phellandrene3. β-Pinene4. Sabinene

5. Myrcene6. Limonene7. γ-Terpinene8. p-Cymene

9. Terpinen-4-ol10. Safrole11. Myristicin

1. C12:02. C14:03. C14:1w54. C16:05. C16:1w7

6. C18:07. C18:1w98. C18:2w69. C18:3w610. C18:3w3

11. C20:012. C20:1w913. C20:2w614. C20:3w915. C20:3w6

16. C20:4w617. C22:018. C22:1w919. C20:5w320. unknown

21. C22:4w622. C24:023. C24:1w924. C22:5w325. C22:6w3

Applications



Analysis of BranchedAlcoholsColumn: TR-WaxMS, 30 m x 0.25 mm

x 0.25 µmPart Number: 260X142PTemperature: 40 °C 5 min, 10 °C/m to 230 °C,

final 230 °CDetector Type: MSCarrrier Gas: He 35 cm/s at 40 °CFlow Rate: 2.3 mL/minInjection 0.1 µLVolume:Injection Mode: Split 100:1, 250 °C

260X017

1. Methanol2. t-Butanol3. i-Propanol4. Ethanol5. i-Butanol6. n-Butanol

7. 2-Methoxyethanol8. 2-Ethoxyethanol9. Propylene glycol10. Ethylene glycol11. Diethylene glycol12. Triethylene glycol

5.00 10.00 15.00 20.00 25.00 30.000

4000000

8000000

1.2e+07

1.6e+07

2e+07

2.4e+07

2.8e+07

1 2

3 4

5

6 7

8

910

1112

13

14

16

15

17

1819

Spearmint OilColumn: TR-WaxMS, 30 m x 0.25 mm x


hold 5 minDetector Type: MSCarrrier Gas: He 25.7 psi, 35cm/sFlow Rate: 1.8 mL/minInjection 0.2 µLVolume:Injection Mode: Split 100:1, 250 °C

260X016

1. α-Pinene2. β-Pinene3. Sabinene4. Myrcene5. Limonene6. 1,8-Cineole7. 3-Octanol8. Menthone9. β-Bourbonene10. L-Linalool

11. trans-caryophyllene12. cis-dihydrocarvone13. trans-dihydrocarvone14. L-Menthol15. Dihydrocarvyl acetate16. L-Carvone17. trans-Carveol18. cis-Carveol19. Caryophyllene oxide

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Food Safety

Notes

316

Documents

Table of Contents Index - Cromlab...2007/12/28 · POROS Becton, Dickinson and Company Luer-LOK Bio-Rad Laboratories, Inc. Aminex Biotage AB EVOLUTE, Isolute Bristol-Myers Squibb