On-Line SPE with the Flexcube/6460 QQQ

Page 1

On-Line SPE with the Flexcube/6460 QQQ

Dr. Sheher Bano Mohsin Mass Spectrometry ApplicationsJune 11, 2013

04/22/20231

Page 2

22.04.20232

•Introduction – Why Online SPE?

•Introducing the Flexcube for Online SPE

•Sensitivity of the Mass Spectrometers

• Application Examples

- Water Samples

- Samples with dirty Matrices

Page 3

22.04.20233

Solid Phase Extraction (SPE)

Wouldn’t it be great if you could automate SPE while reducing sample and solvent volumes?

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22.04.20234

Automated on-line SPE 1. Load 500ul-1800 µl water sample on the enrichment cartridge.

2. Valve switch, ‘backflush‘ desorb using HPLC gradient.

3. Separate on the analytical column and collect MRM tranistions on the QQQ.

4. Recondition enrichment cartridge during analysis.

5. Ready for next sample after ~ 20 minutes.

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22.04.20235

High sensitivity 6460 Triple Quadrupole• Sub-femtogram, on-column sensitivity (1pg reserpine; s/n 2000:1) • Five Orders of Linearity• Fast Pos/Neg switching, 30 millisec• “Dynamic Multiple Reaction Monitoring” for MRMs scheduled by peak

retention times instead of time segments• Triggered MRM for confirmation

Agilent Jet Stream

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22.04.20236

Agilent MassHunter Software

Instrument ControlReal-time monitoring

Method set-up

Autotune

Qualitative AnalysisChromatographic results

Spectral results

Find compounds

Quantitative AnalysisUser filters

Compound results

Calibration curve

Reporting Easily CustomizableBased on Excel and

XML technology

Page 7

22.04.20237

Agilent Online SPE System

Switching valve with TEC

Quaternary pump

Autosampler

Analytical column for separation

Binary pump for gradient elution

MS/MS

Page 8

22.04.20238

WHAT’S NEW WITH ONLINE SPE?

Flexcube with Built in Valves and a Pump - all Controlled

through Mass Hunter

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22.04.20239

Agilent Online SPE System

Switching valve with TEC

Quaternary pump

Autosampler

Analytical column for separation

Binary pump for gradient elution

MS/MS

Replace with Flexcube

Page 10

Agilent 1200 Infinity Series Online SPE solution

Solvent selection valve for up to three solvents

Reciprocating single-piston pump for flows up to 4 ml/min (60 bar)

up to two Quick-Change valves, according to application

10

Valves mounted in 1290 Infinity Flexible Cube

Page 11

Online SPE with the Flex Cube

Autosampler with 900uL loop and extension seat capillary

1290 Binary Pump

1290 Autosampler

Column Compartment

6460 QQQ

Flexcube

Autosampler

Page 12

Flex Cube and Autosampler

Single Piston Pump

6 port valve 10 port valve

Autosampler

Page 13

Mass Hunter B 06.00 with Flexcube Control

Page 14

1260 Bin Pump

System with alternating SPE loading:Load sample to SPE1

SPE2

SPE1

Std. ALS 900 µL head

Flex cube pump Column

waste

Load

SPE starter set

Page 15

1260 Bin Pump

System with alternating SPE loading:Elute sample from SPE1 to column / Load sample 2 on SPE2

SPE2

SPE1

Std. ALS 900 µL head

Flex cube Column

waste

Elute

Load

Mass Spec

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22.04.202316

Application:

Quantitative LC/MS/MS analysis of 24 trace pharmaceuticals and consumer products in water using on-line SPE enrichment.

Tarun Anumol and Shane Snyder University of Arizona

Sheher Mohsin – Agilent Applications Scientist

Page 17

22.04.202317

Compounds AnalyzedCompound Class Compound Class

Atrazine Herbicide PFBS Fluoro-surfactantBisphenol A Plasticizer PFOA Fluoro-surfactant

Caffeine Stimulant PFOS Fluoro-surfactantCarbamazepine Anti-seizure Primidone Anticovulsant

DEET Insect-repellant Simazine HerbicideEstrone Hormone Sulfamethoxazole Antibiotic

Fluoxetine Anti-depressant Atenolol Β-blockerGemfibrozil Anti-cholesterol TCPP Flame-retardantIbuprofen Analgesic Testosterone Hormone

Meprobamate Anti-anxiety Triclocarban Anti-microbialNaproxen Pain-reliever Triclosan Anti-microbialDiltiazem Anti-histamine Trimethoprim Antibiotic

Page 18

22.04.202318

Summary Experimental Methods

1. Collect 5 mL sample and store at 4C for preservation.

2. Filter sample through 0.2 µm filters.

3. Combine 1683 µL of sample (weight using analytical balance for accuracy) with 17 µL of a 10 ppb surrogate standard mix. Vortex for 30 sec.

4. Analyze by UHPLC/MS/MS with the Agilent 1290 LC coupled to an Agilent 6460 Mass Spectrometer LC/MS/MS.

Page 19

Chromatography

04/22/202319

Simultaneous analysis of 24 PPCPs in both ESI+ & ESI- mode.

Injection Volume: 1.5 mL

Cycle time (Extraction + Analysis): 18.5 min

Trace Enrichment Cartridge: PLRP-S, 15 µm

Analytical Column: Poroshell 120 EC, 2.1x50 mm

Page 20

22.04.202320

Analyte MRL Analyte MRL

Atenolol 15 Meprobamate 0.5

Atrazine 5 Naproxen 10

Bisphenol A 10 PFBS 10

Caffeine 0.5 PFOA 10

Carbamazepine 2.5 PFOS 10

DEET 0.1 Primidone 15

Estrone 20 Simazine 1.5

Fluoxetine 10 Sulfamethoxazole 2.5

Gemfibrozil 1.5 TCPP 0.5

Ibuprofen 10 Triclocarban 1

Trimethoprim 5 Triclosan 5

Method Reporting Limits (ng/l)

S/N> 10 (by height) for 3 successive injections

Page 21Confidential21 April 2010

Evaluation of On-line Solid Phase Extraction and Direct Injection-LC/MS/MS for the Analysis of Chemicals on

U.S. EPA’s Contaminant Candidate List 3

Sheher Bano Mohsin

Page 22

Chemicals for LC/MS/MS Evaluation*

•4,4’-methylenedianiline

•3-hydroxycarbofuran

•bensulide

•clethodim

•fenamiphos

•fenamiphos sulfone

•fenamiphos sulfoxide

• methomyl • quinoline• tebuconazole• tebufenozide• thiodicarb

9 CCL3 chemicals 3 CCL3 degradates

*Slide Taken From: Evaluation of On-line Solid Phase Extraction-LC/MS/MS for the Analysis of Chemicals on U.S. EPA’s Contaminant Candidate List 3 - Jody A. Shoemaker and Daniel R. Tettenhorst


Agilent 1200 Infinity Series Online-SPE solution system comprising:G1312B Binary Pump with modular degasserG1329B Standard AutosamplerG4227A Flexible Cube with 2-position/10-port valves, G1316C Thermostatted Column Compartment. 6460 Triple Quadrupole LC/MS with Jet Stream Technology

Online SPE Instrumentation in Schaumburg

Page 24

Configuration showing the plumbing for direct on-column injection and on-line SPE.

Page 25

LC/MS/MS Parameters

Triple Quadruple MS method with Agilent Jet Stream thermal gradient focusing technology:• Gas temperature: 300 °C. Gas flow: 10 L/min.• Nebulizer: 45 psi• Sheath gas temperature: 350 °C. Sheath gas flow: 11 L• Capillary: 4,000 Volt. Nozzle: 0 Volt

Binary Pump:• Solvent A: Water + 0.1% formic acid. • Solvent B: ACN + 0.1% formic acid. Analysis Flow rate: 0.4 mL/min.Column: ZORBAX EclipsePlus C18 3.0x50mm 1.8 μm, 50 °C.Flexible Cube:Valves: 2 of 2-position/10-port Quick-Change valves.Flow rate: 1.0 mL/min. Solvent: A1: 3% MeOH/Water, B1: ACN/IPA/MeOH/Water 1/1/1/1 v/v/v/v.Standard Autosampler fitted with 900 μL metering headAuto-SPE Injection volume: 900 μL using a draw and eject speed of 1,000 μL/min. Direct Injection volume: 90 μL

Page 26

Cmpd Name Prec Ion

Prod Ion

Frag (V)

CE (V) Cell Acc (V)

Ret Time (min)

Ret Window

Polarity

4-4-diaminodiphenylmethane

199.1 106 120 28 3 6.74 1.81 Positive

Bensulide 398 356 100 1 2 11.06 1.11 PositiveBensulide 398 314 100 6 2 11.06 1.11 PositiveBensulide 398 158 100 26 2 11.06 1.11 Positive

Carbofuran-3-hydroxy 238.1 181 110 8 2 8.15 0.94 PositiveCarbofuran-3-hydroxy 238.1 163 110 11 2 8.15 0.94 Positive

Clethodim 360.1 206 120 12 4 11.67 1.15 PositiveClethodim 360.1 166 130 27 4 11.67 1.15 Positive

Fenamiphos 304.1 234 150 15 3 10.28 1.03 PositiveFenamiphos 304.1 217 150 23 3 10.28 1.03 PositiveFenamiphos 304.1 202 150 31 3 10.28 1.03 Positive

Fenamiphos-sulfone 336.1 308 130 15 3 9.13 0.91 PositiveFenamiphos-sulfone 336.1 266 130 18 3 9.13 0.91 PositiveFenamiphos-sulfone 336.1 188 130 24 3 9.13 0.91 Positive

Fenamiphos-sulfoxide 320.1 292 150 9 3 8.64 0.99 PositiveFenamiphos-sulfoxide 320.1 233 150 23 3 8.64 0.99 PositiveFenamiphos-sulfoxide 320.1 171 150 18 3 8.64 0.99 Positive

Methomyl 163 107 170 17 2 8.15 1.14 PositiveMethomyl 163 95 170 17 2 8.15 1.14 PositiveQuinoline 130 103 120 30 3 6.97 1.81 PositiveQuinoline 130 77 120 30 3 6.97 1.81 Positive

Tebuconazole 308.1 125 130 42 3 10.49 1.05 PositiveTebuconazole 308.1 70 130 23 3 10.49 1.05 PositiveTebufenozide 353.2 297 85 1 3 10.85 1.09 PositiveTebufenozide 353.2 133 85 15 3 10.85 1.09 Positive

Thiodicarb 355 163 80 2 3 9.17 1.28 PositiveThiodicarb 355 108 80 14 3 9.17 1.28 PositiveThiodicarb 355 88 80 17 3 9.17 1.28 Positive

Dynam

ic MR

M Transitions

Page 27

5x10

00.10.20.30.40.50.60.70.80.9

11.11.21.31.41.51.6

+ESI TIC MRM CF=0.000 DF=0.000 (** -> **) 10ppt-r002.d 1 1

Counts vs. Acquisition Time (min)6 6.5 7 7.5 8 8.5 9 9.5 10 10.5 11 11.5 12

Superimposed chromatograms Showing Reproducibility of Retention time as well as Area Counts for two runs Alternating Between two Different SPE Cartridges. The calibration standard used has a concentration of 10 ppt (ng/L) each for all 12 compounds with quantifier and qualifier ions. Each run alternates between two different SPE cartridges.

Page 28

Mix at 1 ppt

3x10

00.10.20.30.40.50.60.70.80.9

11.1

+ESI MRM Frag=100.0V CF=0.000 DF=0.000 [email protected] (398.0000 -> 356.0000) 1ppt-r001.d 11.0481 1

Counts vs. Acquisition Time (min)6 6.2 6.4 6.6 6.8 7 7.2 7.4 7.6 7.8 8 8.2 8.4 8.6 8.8 9 9.2 9.4 9.6 9.8 10 10.2 10.4 10.6 10.8 11 11.2 11.4 11.6 11.8 12

Fenomiphos Sulfoxide

Fenomiphos Sulfone

Tebufenozide

Thiodicarb

Clethodim

Bensulide

Tebuconazole

Fenomiphos

Carbofuran-3-Hydroxy

Methomyl

Quinoline

4,4-diaminodiphenyl methane

Page 29

Mix at 0.1 ppt

2x10

00.5

11.5

22.5

33.5

44.5

55.5

66.5

+ESI MRM Frag=100.0V CF=0.000 DF=0.000 [email protected] (398.0000 -> 356.0000) 0-1ppt-r002.d

11.042

1 1

Counts vs. Acquisition Time (min)6 6.2 6.4 6.6 6.8 7 7.2 7.4 7.6 7.8 8 8.2 8.4 8.6 8.8 9 9.2 9.4 9.6 9.8 10 10.2 10.4 10.6 10.8 11 11.2 11.4 11.6 11.8 12

Page 30

1 ppt and 0.1 ppt

3x10

00.20.40.60.8

11.21.41.61.8

22.22.42.6

+ESI MRM Frag=130.0V CF=0.000 DF=0.000 [email protected] (336.1000 -> 266.0000) 0-1ppt-r002.d

9.123

1

Counts vs. Acquisition Time (min)7.4 7.6 7.8 8 8.2 8.4 8.6 8.8 9 9.2 9.4 9.6 9.8 10 10.2 10.4 10.6 10.8 11 11.2 11.4 11.6 11.8 12

1 ppt

0.1 ppt 1 ppt

0.1 ppt

1ppt

0.1 ppt

1 ppt

0.1 ppt

1 ppt

0.1 ppt

Page 31

Direct Injection and online-SPESame amount on column

4x10

0

2

4

6

8

+ESI TIC MRM CF=0.000 DF=0.000 (** -> **) 50-direct-r002b.d 1 1

4x10

0

2

4

6

8

+ESI TIC MRM CF=0.000 DF=0.000 (** -> **) 5ppt-r002.d 1 1

Counts vs. Acquisition Time (min)1.5 2 2.5 3 3.5 4 4.5 5 5.5 6 6.5 7 7.5 8 8.5 9 9.5 10 10.5 11 11.5 12

Direct Injection

Online SPE

Page 32

Fenomiphos Sulfoxide

2x10

0.5

1

1.5

2

2.5

3

3.5

4

+ESI MRM Frag=150.0V CF=0.000 DF=0.000 [email protected] (320.1000 -> 171.0000) 0-1ppt-r001.d Noise (RMS) = 14.76; SNR (8.635min) = 8.2

1218.635

Counts vs. Acquisition Time (min)7.8 8 8.2 8.4 8.6 8.8 9 9.2 9.4 9.6 9.8 10 10.2 10.4 10.6

0.1 ppt

0.5 ppt

1.0 ppt

Page 33

Fenomiphos Sulfoxide0.1 ppt to 100 ppt

On-line SPE

Fenamiphos-sulfoxide - 7 Levels, 7 Levels Used, 14 Points, 14 Points Used, 0 QCs

Concentration (pg/ml)-5 0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 105

Resp

onse

s 5x10

-0.250

0.250.5

0.751

1.251.5

1.752

2.252.5

2.753

3.253.5

3.754

4.254.5

4.75

y = 4783.281270 * x - 1547.513777R^2 = 0.99976373Type:Linear, Origin:Ignore, Weight:None

Page 34

Fenomiphos Sulfone

2x10

0.5

1

1.5

2

2.5

3

3.5


1399.134


1 ppt

0.5 ppt

0.1 ppt

Page 35

Fenomiphos Sulfone 0.1 ppt to 100 ppt

Online -SPE

Fenamiphos-sulfone - 7 Levels, 7 Levels Used, 14 Points, 14 Points Used, 0 QCs


Resp

onse

s 5x10

-0.5-0.25

00.250.5

0.751

1.251.5

1.752

2.252.5

2.753

3.253.5

3.754

4.254.5

4.755

5.25

y = 5253.702203 * x - 554.970972R^2 = 0.99622328Type:Linear, Origin:Ignore, Weight:1/x

Page 36

Tebufenozide

3x10

0

0.2

0.4

0.6

0.8

1

1.2

1.4

1.6

1.8


10.848

Counts vs. Acquisition Time (min)9.2 9.4 9.6 9.8 10 10.2 10.4 10.6 10.8 11 11.2 11.4 11.6 11.8

1 ppt

0.5 ppt

0.1 ppt

Page 37

Tebufenozide

Online SPE

Tebufenozide - 7 Levels, 7 Levels Used, 14 Points, 14 Points Used, 0 QCs


Resp

onse

s 6x10

-0.1

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1

1.1

1.2

1.3

1.4

1.5

1.6


Page 38

Thiodicarb

2x10

0.5

1

1.5

2

2.5

3

3.5


9.167

Counts vs. Acquisition Time (min)7.4 7.6 7.8 8 8.2 8.4 8.6 8.8 9 9.2 9.4 9.6 9.8 10

Page 39

Thiodicarb

Online SPE

Thiodicarb - 7 Levels, 7 Levels Used, 14 Points, 14 Points Used, 0 QCs


Resp

onse

s 6x10

-0.050

0.050.1

0.150.2

0.250.3

0.350.4

0.450.5

0.550.6

0.650.7

0.750.8

0.850.9

0.951


Page 40

Clethodim

2x10

0.4

0.6

0.8

1

1.2

1.4

1.6

1.8


* 11.678

1


Page 41

Clethodim0.1 ppt to 100 ppt

Online-SPE

Clethodim - 7 Levels, 7 Levels Used, 14 Points, 14 Points Used, 0 QCs


Resp

onse

s 4x10

-0.5

0

0.5

1

1.5

2

2.5

3

3.5

4

4.5

5

5.5

6

6.5

7y = 671.580771 * x - 96.141931R^2 = 0.99912930Type:Linear, Origin:Ignore, Weight:None

Page 42

Bensulide

2x10

0.5

1

1.5

2

2.5

3

3.5

4

4.5

5


11.064

1


1 ppt

0.5 ppt

0.1 ppt

Page 43

Bensulide

Online SPE

Bensulide - 7 Levels, 7 Levels Used, 14 Points, 14 Points Used, 0 QCs


Resp

onse

s 5x10

-0.5

0

0.5

1

1.5

2

2.5

3

3.5

4

4.5

5

5.5

6y = 5847.762254 * x - 167.472128R^2 = 0.99942301Type:Linear, Origin:Ignore, Weight:None

Page 44

Tebuconazole

4x10

0

0.2

0.4

0.6

0.8

1

1.2

1.4


10.484

Counts vs. Acquisition Time (min)10 10.1 10.2 10.3 10.4 10.5 10.6 10.7 10.8 10.9 11

1 ppt

0.5 ppt

0.1 ppt

Page 45

Tebuconazole0.1 ppt to 100 ppt

Online SPE

Tebuconazole - 7 Levels, 7 Levels Used, 14 Points, 14 Points Used, 0 QCs


Resp

onse

s 6x10

-0.2

0

0.2

0.4

0.6

0.8

1

1.2

1.4

1.6

1.8

2

2.2

2.4

2.6

2.8

3y = 29206.177838 * x + 9683.405016R^2 = 0.99961760Type:Linear, Origin:Ignore, Weight:None

Page 46

Fenomiphos

3x10

0

0.2

0.4

0.6

0.8

1

1.2

1.4

1.6

1.8


10.278

Counts vs. Acquisition Time (min)9.2 9.4 9.6 9.8 10 10.2 10.4 10.6 10.8 11 11.2

1 ppt

0.5 ppt

0.1 ppt

Page 47

Fenomiphos

Online SPE

Fenamiphos - 7 Levels, 7 Levels Used, 14 Points, 14 Points Used, 0 QCs


Resp

onse

s 6x10

-0.2

0

0.2

0.4

0.6

0.8

1

1.2

1.4

1.6

1.8

2

2.2

2.4


Page 48


3x10

0

0.5

1

1.5

2

2.5

3

3.5

4

4.5


8.143

1

Counts vs. Acquisition Time (min)3.5 4 4.5 5 5.5 6 6.5 7 7.5 8 8.5

1 ppt

0.5 ppt

0.1 ppt

Page 49


Online SPE

Carbofuran-3-hydroxy - 7 Levels, 7 Levels Used, 14 Points, 14 Points Used, 0 QCs


Resp

onse

s 6x10

-0.1

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1

1.1

1.2

1.3

1.4

y = 14014.214494 * x + 12281.460374R^2 = 0.99789149Type:Linear, Origin:Ignore, Weight:None

Page 50

Quinoline

4x10

0

1

2

3

4

5

6

7


6.972

1

Counts vs. Acquisition Time (min)4 4.5 5 5.5 6 6.5 7 7.5 8 8.5

1 ppt

0.5 and 0.1 ppt

Page 51

Quinoline0.1 to 1000 ppt

Online SPE

Quinoline - 10 Levels, 10 Levels Used, 18 Points, 18 Points Used, 0 QCs

Concentration (pg/ml)0 100 200 300 400 500 600 700 800 900 1000

Resp

onse

s 6x10

-0.4-0.2

00.20.40.60.8

11.21.41.61.8

22.22.42.62.8

33.23.43.63.8

44.24.4

y = 4212.447667 * x + 37135.461218R^2 = 0.96037929Type:Linear, Origin:Ignore, Weight:1/x

Page 52

Water Samples Analysis

Water samples from a lake-fed municipal water supply (tap), residential well (ground), a suburban collection basin (WestLake) and a flood control reservoir (Spring Creek) were analyzed. Notably, both WestLake and Spring Creek are in the drainage basin of nearby public and private golf courses.

Samples were filtered with 0.45 um disk filters prior to analysis.

Page 53

Tebuconazole in Water

5x10

0

0.5

1

1.5

2

2.5

3

3.5

4

4.5

+ESI TIC MRM CF=0.000 DF=0.000 (** -> **) filtered Westlake1.d

Counts vs. Acquisition Time (min)6.5 7 7.5 8 8.5 9 9.5 10 10.5 11

Spring Creek 50 ppt

WestLake 37 ppt

Ground 0.9 ppt

Tap 0.004 ppt

Page 54

Lake Water and Ground water

5x10

0

0.5

1

1.5

2

2.5

3

3.5

4

4.5

5

+ESI MRM Frag=130.0V CF=0.000 DF=0.000 [email protected] (308.1000 -> 70.0000) filtered Westlake1.d 1

Counts vs. Acquisition Time (min)8 8.5 9 9.5 10 10.5 11 11.5 12

Ground Water

Lake Water

Amount ~ 50 ppt

Results are based on the average of duplicate analyses, for the one quantifier transition (308.1 to 70.0) and one qualifier transition (308.1 to 125.0). Tebuconazole is used as a fungicide for turf control. Both WestLake and Spring Creek are in the drainage basin of nearby public and private golf courses.

Page 55

Compound Name Level (ppt) Signal to Noise (S/N)

Nominal LOQ @ 10:1 S/N

4-4-diaminodiphenylmethane

0.1 25 0.04

Bensulide 0.1 10.3 0.1Carbofuran-3-hydroxy 0.1 34.4 0.03

Clethodim 0.1 7 0.15Fenamiphos 0.1 301.2 0.005

Fenamiphos-sulfone 0.1 7.9 0.15Fenamiphos-sulfoxide 0.1 8.2 0.15

Methomyl 0.1 8.3 0.15Quinoline* 0.1 500 0.002

Tebuconazole 0.1 427 0.0025Tebufenozide 0.1 9.4 0.15

Thiodicarb 0.1 9 0.15* uncertainty due to unresolved carryover

Performance data for all compounds present in the study based on the calculated signal to noise at 0.1 ppt and assuming an LOQ at approximately 10: 1 signal-to-noise. The signal to noise calculation is based on peak area and noise is RMS x 3.

Page 56Confidential56

Trace level analysis of herbicides in drinking and surface water by online-SPE LC/triple quadruploe MS to the lower ppt rangeEdgar Naegele, Agilent Technologies R&D and Marketing GmbH & Co. KG, Waldbronn, Germany

April 2010


MRM and dynamic MRM MS method


Chromatograms of a calibration standard with a concentration of 100 ppt (ng/L) each for all 28 pesticides measured by the final SPE-LC dynamic MRM method with quantifier and

qualifier ion.


Water samples from a tap, Rhine river, and a spring spiked with 25 ppt of all 28 pesticides. The retention time window from 14.5 minutes to 19.1 minutes is shown. The table shows the average measured concentrations of all pesticides (n=12) within the retention time window dependent on the sources of water together with precision RSD and accuracy.

Page 60

Conclusions

We have demonstrated an integrated, cost effective scheme to do on-line SPE coupled to LC/MS/MS. The technical barriers and potential technology transfer problems associated with traditional online SPE system have been avoided.The direct coupling of the SPE cartridges (PLRP-S, 2.1x12.5mm, 15-20um) to the LC/MS/MS system was done through the integrated valves. The use of Dynamic MRM enables complex mixtures to be efficiently analyzed.

We have demonstrated excellent performance with challenging contaminants on the contaminant list. LOQ for all components was nominally 1 ppt or lower.

Results for real samples, including ground water, lake and flood control reservoir, the latter two obviously containing visible swimming organisms, produced measurable tebuconazole results.

Page 61

Agilent 1200 Infinity Series Online SPE solution

61

Expand Your Versatility

• Boost Performanceenrichment of analytes and matrix removal for utmost sensitivity

• Save Timeindividual configurations for broad automation flexibility

• Reduce Costs1290 Infinity Flexible Cube contains a built-in pump

For online sample preparation, upgrade your system with Agilent 1290 Infinity Flexible Cube featuring

• built-in pump to condition and flush re-usable cartridges

• solvent selection valve

Page 62Confidential62

Journal of Chromatography A, 1286 (2013) 166– 174Quantitative analysis of naphthenic acids in water by liquid chromatography–accurate mass time-of-flight mass spectrometry

Ralph Hindle, Matthew Noesthedena, Kerry Perub, John Headley

Vogon Laboratory Services Ltd., Unit 4, 34 Griffin Industrial Pt., Cochrane, Alberta T4C 0A3, Canada

Water Science & Technology Directorate, Environment Canada, 11 Innovation Blvd., Saskatoon, SK S7N 3H5, Canada

April 2010

Documents

On-Line SPE with the Flexcube/6460 QQQ