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Issue 1 • 2016
Glyphosate and GlufosinateCertified Reference Materials
pg. 3
Extracts of Plant Materials
Marine Biotoxin CRMs
Flavors and Fragrances Testing
NIST Reference Materials
Isotope Labeled Pesticides
Carotenoid Standards
Feature Article3 Glyphosate and Glufosinate-ammonium Now Available
as TraceCERT® Grade Several New Organic Certified Reference Materials Added
Standards4 Standards for Single Components and
Extracts of Medicinal PlantsNew Primary and Secondary Pharmaceutical Standards from HWI Analytik
6 Marine Biotoxin CRMsProducts from the National Research Council of Canada (NRC) Now Available through Sigma-Aldrich®
7 Flavors and Fragrances Portfolio Keeps GrowingNEW Standards for Aroma Compounds for Food and Cosmetics Analysis
8 NIST Reference Materials and Standard Reference Materials® for Environmental and Food AnalysisUpdate on the Product Launch
11 NEW Isotope Labeled Pesticide StandardsComplementing the Sigma-Aldrich® Comprehensive Range of Pesticide Standards
12 Neoxanthin and Other CarotenoidsNew Analytical Standards for Food Testing
13 NEW Certified Reference Materials for ISO Method 17943
14 Products from Jaytee® Now at Sigma-Aldrich®Kromega Range of Qualification Standards
16 ULTRA100 Certified Low Level TOC VialsFrom Dual Accredited Producer Altus Science
Labware 17 Timestrip®
The Smart Way to Measure Time and Temperature
Chromatography 18 Ion-Pair Chromatography of Phosphorylated
Sugar Metabolites
Michael Jeitziner
Dear Customer,
Sigma-Aldrich® offers a wide range of analytical products to meet your needs including reagents and reference materials for chromatography, electrochemistry, spectroscopy, titration, microbiology and wet chemistry.
We are proud to announce the recent release of our new web portals for key analytical product lines:
Sigma-Aldrich offers close to 20,000 analytical standards and certified reference materials (CRMs), as well as OEM and custom
products and services. Our newly designed faceted navigation basically extends the idea of filtering even further into a complex structure of chemical classes, applications, methods, and other search criteria. It allows searchers to continually narrow down their results by clicking another constraint in their search.
Explore our new portal for analytical standards and certified reference materials at sigma-aldrich.com/standardsISO/IEC 17025 accredited laboratories are required to take part in proficiency testing (PT) programs to demonstrate performance and method validation. Sigma-Aldrich has launched a new portal for proficiency testing services at sigma-aldrich.com/ptFinally, I invite you to explore our new analytical reagents and solvents portals at sigma-aldrich.com/analytical-reagents. You can quickly find the analytical reagent, buffer, or solvent you need to run your analytical application.
With kind regards,
Michael Jeitziner Senior Marketing Manager Analytical Reagents & Standards [email protected]
New Web Portals – Convenient Navigation through Sigma-Aldrich’s Analytical Reagents & Standards Offering
Analytix is published five times per year by Sigma-Aldrich Chemie GmbH, Industriestrasse 25, CH-9471 Buchs SG, Switzerland.Sigma-Aldrich Corp. is a subsidiary of Merck KGaA, Darmstadt, Germany. Publisher: Sigma-Aldrich Marketing Operations Europe Publication Manager: Michael Jeitziner Editor: Daniel Vogler
sigma-aldrich.com/analytix 2
3Feature Article
Matthias Nold, Product Manager Analytical Standards [email protected]
Alexander Rück, Supervisor R&D Europe [email protected]
Christine Hellriegel, Senior Scientist R&D Europe [email protected]
TraceCERT® organic neat CRMs (certified reference materials) are developed and manufactured at our site in Buchs, Switzerland, under ISO/IEC 17025 and ISO Guide 34 double accreditation. To date, more than 200 of these high quality products have become available, providing our analytical customers with traceable certified reference materials of the most relevant analytes for food, cosmetics and environmental testing (sigma-aldrich.com/organiccrm).
The main characteristics of organic TraceCERT certified reference materials are:
• Certified content by high performance quantitative NMR (HP-qNMR)
• Compliant to ISO/IEC 17025 and ISO Guide 34
• Superior level of accuracy, calculated uncertainties, and lot-specific values
• Traceability to NIST SRM
• Comprehensive documentation delivered with the product (certification according to ISO Guide 31)
The use of quantitative NMR (qNMR) as a relative primary analytical method using internal standards, which are traceable to NIST SRM, enables us to establish traceable, quantitative values for almost every organic compound. Because the values of the integrals of the proton signals are not affected by the chemical structure, qNMR allows quantitative comparison between different organic molecules, which is not possible with most other analytical techniques. If you are interested in learning more about quantitative NMR, please refer to the references [1–3] noted below or contact us.
New products are continually added to the range. The most recent product additions include Glyphosate and Glufosinate-ammonium, two of the most widely used herbicides. The mode of action of both of these organophosphorus herbicides is the inhibition of an enzyme of the amino acid biosynthesis in plants without affecting the metabolisms of humans or animals.
Also among the new products is 4,4’-Diaminodiphenylmethane (MDA), a chemical used in the process of polyurethane production and which has been added to the “substances of very high concern”
(SVHC) list of the European Chemicals Agency (ECHA) due to its suspected carcinogenicity.
Additional new products include dyes (Leucomalachite Green), preservatives (Butylated hydroxyanisole, Diisopropyl phthalate) or flavors (Isobutyric acid) among others, which reflects the broad range of analytes that are covered by the organic TraceCERT CRMs.
Cat. No. Description Package Size49886 Butylated hydroxyanisole 50 mg69630 Butyraldehyde-2,4-DNPH 50 mg18139 4,4'-Diaminodiphenylmethane (MDA) 50 mg91009 Diisopropyl phthalate 50 mg16902 Diuron 50 mg49677 Glufosinate-ammonium 100 mg89432 Glyphosate 100 mg96499 Isobutyric acid 100 mg78567 Leucomalachite green 25 mg15633 Pefabloc SC 50 mg42681 2-Phenylethylamine 50 mg
Glyphosate and Glufosinate-ammonium Now Available as TraceCERT® GradeSeveral New Organic Certified Reference Materials Added
Table 1 Most Recent Additions to the TraceCERT Product Range
References:[1] TraceCERT® Organic Certified Reference Materials, Analytix, Vol 3 2010;
Vol. 1 2011; Vol. 3 2011; Vol 4 2011.[2] TraceCERT® Organic Certified Reference Materials, Analytix, Vol 2 2010[3] Weber M.; Hellriegel C.; Rück A.; Sauermoser R.; Wüthrich J. Using high-
performance quantitative NMR (HP-qNMR (R)) for certifying traceable and highly accurate purity values for organic reference materials with uncertainties < 0.1 % Accred. Qual. Assur (2013), Volume 18, Issue 2, pp 91–98.
3
NH2H2N
H3C PO
OH NH2
ONH4
O
HO PO
OH
HN
OH
O
Glyphosate
4,4’-Diaminodiphenylmethane (MDA)
Glufosinate-ammonium
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Analytix | 1: 2016 4
sigma-aldrich.com/analytixsigma-aldrich.com/medicinalplants
Standards for Single Components and Extracts of Medicinal PlantsNew Primary and Secondary Pharmaceutical Standards from HWI Analytik
Matthias Nold, Product Manager Analytical Standards
In January 2011, we launched the first series of primary pharmaceutical standards designed for the testing of herbal medicinal products. These products are manufactured by HWI Analytik in Rülzheim (Germany) and exclusively distributed by Sigma-Aldrich® [1]. After the enthusiastic reception of these standards by our customers, the range was continually expanded and currently consists of more than 120 products. Table 1 shows the newest additions, and a complete listing can be found online at sigma-aldrich.com/phytopharma
The content value of these products is determined by quantitative NMR (qNMR) [2]. This technique is increasingly applied in the chemical and pharmaceutical industries as a direct relative method to quantify organic compounds. It is a very convenient alternative to the mass balance approach, which calculates the content by measuring all potential impurities and subtracting them from 100%. Particularly for natural products isolated from plants, the mass balance approach is very challenging.
In addition to the quantitative NMR value, the certificate delivered with these products also contains a chromatographic purity value.
Quantitative NMR is also applied by Sigma-Aldrich for the certification of the organic TraceCERT® products [3] (see also the article on page 3 of this issue of Analytix).
.
Cat. No. Description Package Size05320590 p-Anisaldehyde 50 mg02890590 β-Asarone 25 mg00400585 (−)-Bornyl acetate 50 mg05330590 Carnosic acid 10 mg03200595 p-Coumaric acid 50 mg05340590 Daidzein 50 mg05370590 Daidzin 10 mg05350590 Ellagic acid 50 mg05360590 Genistein 50 mg05380590 Genistin 25 mg00960590 Isorhamnetin-3-O-β-D glucopyranosyl-
(12)-β-D glucopyranosyl-(16)-β-D glucopyranoside
10 mg
05390590 Myricetin 10 mg05400590 Oleuropein 10 mg05410590 Salidroside 10 mg02090580 β-Sitosterol 10 mg05420590 Stevioside 25 mg
Table 1 New additions of Primary Pharmaceutical Reference Standards of Phytochemicals
b-Asarone
Isorhamnetin-3-O-β-D glucopyranosyl-(1-2)-β-D glucopyranosyl-(1-6)-β-Dglucopyranoside
Salidroside
Figure 1 Chemical Structures of Some New Primary Pharmaceutical Reference Standards
4
H
CH3
OCH3
OCH3
OCH3H
O
OH
HO
OO
OCH3
OH
O
OH
OH
OH
OO
O
OH
OH
HO
O
OH
OH
OH
HOO
OH
OHOH
HOO
OH
Back to Table of Contents
5Feature ArticleStandards
Cat. No. Description Package Size05495001 Camellia sinensis extract 150 mg05485001 Ginkgo biloba extract 150 mg05475001 Senna extract 150 mg
Table 2 New Plant Extract Reference Materials
The standards from HWI Analytik represent the premium quality of our product range of standards and reference materials for ingredients of medicinal herbs, comprising more than 500 products. A complete list can be found at sigma-aldrich.com/medicinalplants. There you can also find a downloadable PDF of the comprehensive Phytochemical Standards brochure containing product listings and chromatographic applications. A hard copy of the brochure can be ordered at sigma-aldrich.com/lit-request
References:[1] Förster G.; Michel F.; Nold M. Analytix 1/2010, 11.[2] Veith M. Analytix 1/2010, 14. [3] Hellriegel C.; Rück A. Analytix 1/2015, 6. [4] Nold M. Analytix 4/2015, 6.
Plant Extract Reference MaterialsTo complement the primary pharma standards of isolated plant ingredients in pure form, last fall we launched a first series of plant extract reference materials [4]. With these products, we provide our customers with real life samples of GMP plant extracts, with quantitative values for one or several key ingredients. The quantitative values are determined by comparison with the corresponding HWI primary pharmaceutical standards. In addition, several other key ingredients are qualitatively confirmed and given as peak assignments in the chromatogram (Figure 1) delivered with the product (including the corresponding chromatographic method).
The first series of seven extracts (visit sigma-aldrich.com/plantextracts for a complete product listing) is now complemented by three new products, listed in Table 2, including camellia sinensis (green tea, chromatogram see Figure 2).
Figure 2 Chromatogram and Certified Values of Camellia Sinensis Extract 05495001
5
Attachment to Certificate of Analysis
page 2 of 2
Figure 1: Chromatogram of Camellia sinensis extract, batch HWI01569
Figure 2: Chromatogram of primary reference standard Epigallocatechin gallate, batch
HWI001521
Grüntee Extrakt, HWI01569 Precision -1-HPLC separating system 1
Project Name Referenzsubstanzen\Extrakte_SiAl_140813\Grüntee_150812SampleName mah15-01444-53 Date Acquired 14.08.2015 17:52:34 CESTVial 10 Acq Method Set All_DAD_2_MSInjection 5 Acquired By HeiterInjection Volume 20,00 ul Date Processed 17.08.2015 12:57:25 CESTRun Time 35,0 Minutes Processing Method TS1_Grüntee_PMSystem Name Alliance 19_2996 Processed By HeiterColumn_No B0811 Result Id 1574Processed Channel Descr. PDA 267,0 nm
Epig
allo
cate
chin
Cat
echi
n
Epica
tech
in
Epig
allo
cate
chin
gal
lat
Epica
tech
in g
alla
te
AU
0,00
0,20
0,40
0,60
0,80
1,00
1,20
1,40
1,60
1,80
2,00
2,20
2,40
2,60
2,80
3,00
Minutes0,00 5,00 10,00 15,00 20,00 25,00 30,00 35,00
1
2
3
4
5
Name RT Area % Area
Epigallocatechin
Catechin
Epicatechin
Epigallocatechin gallat
Epicatechin gallate
6,553
8,009
9,705
12,965
16,754
1936371
169307
1752183
25838213
6269160
5,384
0,471
4,872
71,842
17,431
Peak Results
Epigallocatechin gallat, HWI01521 PS-1-HPLC separating system 1
Project Name Referenzsubstanzen\Extrakte_SiAl_140813\Grüntee_150812SampleName mah15-01444-95 Date Acquired 17.08.2015 18:53:48 CESTVial 36 Acq Method Set All_DAD_2_MSInjection 1 Acquired By HeiterInjection Volume 20,00 ul Date Processed 18.08.2015 08:54:28 CESTRun Time 35,0 Minutes Processing Method TS1_Grüntee_PMSystem Name Alliance 19_2996 Processed By HeiterColumn_No B0811 Result Id 1735Processed Channel Descr. PDA 267,0 nm
Epig
allo
cate
chin
gal
lat
AU
0,00
0,20
0,40
0,60
0,80
1,00
1,20
1,40
1,60
1,80
Minutes0,00 5,00 10,00 15,00 20,00 25,00 30,00 35,00
1
2
3
4
5
Name RT Area % Area
Epigallocatechin
Catechin
Epicatechin
Epigallocatechin gallat
Epicatechin gallate
6,649
8,007
9,741
12,994
16,792
23037996 100,000
Peak Results
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Analytix | 1: 2016 6
sigma-aldrich.com/analytix
New Certified Reference Materials for Marine Biotoxins
Manufactured by the National Research Council of Canada (NRC)Provided as CRM Solutions or Matrix Materials sigma-aldrich.com/marinetoxins
6
Inorganic Custom StandardsAn Interactive Online Platform
With a few simple mouse clicks you can definethe standard you need choosing between elementstandard and ion standard, defining matrix, analytesand concentrations.
The new Custom Standards Platform is a dynamicweb page: elements, ions and matrices can only bechosen if the combinations are chemically allowed.
After your request has been submitted online, wewill evaluate the production costs and come back to you with a quotation by e-mail.
It’s easy, try it out!
*At www.sigma-aldrich.com/tracecert you canfind the extensiveTraceCERT portfolio of certified single- and multi-element standards.
TraceCERT® standards for AAS, ICP and IC areCertified Reference Materials fulfilling the highest-quality standards.* Now we can also offer you acustom service where you can define your own multi-component standards at the same high quality, usingour NEW Inorganic Custom Standards Online Platform:
www.sigma-aldrich.com/csp
For all TraceCERT Custom Standards we guarantee:
• Certification under double accreditation following ISO/IEC 17025 and ISO Guide 34• Highest level of accuracy and reliability• Minimised uncertainties and lot specific values• Traceability to at least two independent references (i.e. NIST, BAM or SI unit kg)• Printed certificate according to ISO Guide 31 • Light- and gas-tight aluminium foil bag packaging allowing up to four years' shelf life
!CSP_Flyer_v6_8.5x11.indd 1 1/26/10 2:17 PM
Inorganic Custom Standards Manufactured under ISO/IEC 17025 and ISO Guide 34 AccreditationAn Interactive Online Platform
With a few simple mouse clicks, you can define your own multi-component standards for ICP and IC in TraceCERT® quality, using our Inorganic Custom Standards Online Platform:
sigma-aldrich.com/csp
Back to Table of Contents
7Feature Article
Matthias Nold, Product Manager Analytical Standards
Sigma-Aldrich® is continually expanding its product offering of analytical standards and certified reference materials (CRMs) of flavors and fragrances for studies and quality control of food, beverages, and cosmetic products.
The current portfolio comprises more than 500 products. In the past few months, over 50 new products have been added, as listed below.
Standards
Flavors and Fragrances Portfolio Keeps GrowingNEW Standards for Aroma Compounds for Food and Cosmetics Analysis
Cat. No. Description Package Size54730 6-Acetyl-1,1,2,4,4,7-hexamethyltetralin 100 mg74394 2-Acetyl-5-methylfuran 250 mg55289 Allyl phenylacetate 1 mL44041 Amyl salicylate 250 mg87894 α-Amylcinnamyl alcohol 500 mg73002 Butyl stearate 1 mL16704 Butyrophenone 1 mL68546 trans-Cinnamyl butyrate 1 mL16976 β-Cyclocitral 1 mL12301 (Z)-β-Damascone 100 mg41163 β-Damascone 250 mg55524 1-Decen-3-ol 1 mL91309 trans-2-Decenal 1mL74001 Dibutyl sulfide 1mL
68709 3’,4`-Dimethoxyacetophenone 100 mg
54306 1,4-Dimethoxybenzene 100 mg
44064 Ebanol (3-Methyl-5-(2,2,3-trimethyl-3-cyclopenten-1-yl)-4-penten-2-ol)
250 mg
68291 Ethyl salicylate 1 mL
03629 5-Ethyl-2,3-dimethylpyrazine 1 mL
74139 2-Ethylthiophene 250 mg
53700 Furfuryl sulfide 100 mg
55392 1-Hepten-3-ol 1 mL
74198 trans,trans-2,4-Hexadienal 1 mL
57524 1,3,4,6,7,8-Hexahydro-4,6,6,7,8,8-hexamethylcyclopenta[g]-2-benzopyran
10 mg
68554 γ-Hexalactone 1 mL
41513 2-Hexanol 1 mL
41152 2-Hydroxypyridine 100 mg
96499 Isobutyric acid TraceCERT 100 mg
68658 3,5-Lutidine 1 mL
Cat. No. Description Package Size19432 3,4-Lutidine 1 mL
68223 2,4-Lutidine 1 mL
36357 Malondialdehyde tetrabutylammonium salt
100 mg
16583 2-Mercaptopropionic acid 1 mL
41162 4-Methoxy-2-methyl-2-butanethiol 250 mg
74164 trans-2-Methyl-2-butenal 1 mL
74914 3-Methyl-2-cyclopentenone 250 mg
97597 7-Methyl-2H-1,5-benzodioxepin-3(4H)-one
100 mg
41301 2-Methyl-2-pentenal 1 mL
55381 2-Methyl-2-thiazoline 1mL
16797 3-Methyl-4-(2,6,6-trimethyl-2-cyclohexen-1-yl)-3-buten-2-one
1mL
49659 2-Methylbutyric acid 1mL
69391 6-Methylcoumarin 100 mg
08552 3-Methylcrotonaldehyde 250 mg
74002 2-Methylpiperidine 1 mL
69697 1-Methylpyridinium Iodide 100 mg
74028 6-Methylquinoline 1 mL
41339 trans Oct-3-en-2-one 1 mL
76516 Octane-1,3-diol 100 mg
09207 cis-1,3-Pentadiene 250 mg
68488 Phenethyl isothiocyanate 250 mg
55528 Phenylacetone 1 mL
44784 Propyl mercaptan 1 mL
75012 3-Propylidenephthalide 1 mL
69791 β,β,3-Trimethylbenzenepropanol 250 mg
61852 Vanillyl alcohol 100 mg
72999 Viridiflorol 25 mg
Table 1 New Flavor and Fragrance Standards
Find the complete portfolio and download the Sigma-Aldrich Flavor and Fragrance Standards brochure on our website at sigma-aldrich.com/flavor
7
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Analytix | 1: 2016 8
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NIST Reference Materials and Standard Reference Materials® for Environmental and Food AnalysisUpdate on the Product Launch
Jens Boertz, Product Manager Analytical Reagents
The National Institute for Standards and Technology (NIST) is one of the oldest physical science laboratories in the U.S. The U.S. Congress established the agency to remove a major handicap to U.S. industrial competitiveness at the time – a second-rate measurement infrastructure that lagged behind the capabilities of England, Germany, and other economic rivals.
Environmental Reference Materials and Standard Reference Materials®
Cat. No. Description Package SizeNIST1515 Apple leaves NIST SRM 1515 50 gNIST1547 Peach leaves NIST SRM 1547 50 gNIST1566B Oyster tissue NIST SRM 1566b 25 gNIST1575A Trace elements in pine needles NIST SRM 1575a 50 gNIST1598A Inorganic constituents in animal serum NIST SRM 1598a 2 vialsNIST1634C Trace elements in fuel oil NIST SRM 1634c 100 mLNIST1640A Trace elements in natural water NIST SRM 1640a 250 mLNIST1646A Estuarine sediment NIST SRM 1646a 70 gNIST1648A Urban particulate matter NIST SRM 1648a 2 gNIST1649B Urban dust NIST SRM 1649b 2 gNIST1650B Diesel particulate matter NIST SRM 1650b 200 mgNIST1941B Organics in marine sediment NIST SRM 1941b 50 gNIST1944 New York/New Jersey waterway sediment NIST SRM 1944 50 gNIST1946 Lake Superior fish tissue NIST SRM 1946 5 x 7-9 g
NIST2260A Aromatic hydrocarbons in toluene NIST SRM 2260a 5 x 1.2 mL
NIST2262 Chlorinated biphenyl cogeners in isooctane NIST SRM 2262 5 x 1.2 mL
NIST2581 Powdered paint NIST SRM 2581, nominal 0.5% lead 35 g
NIST2583 Trace elements in indoor dust NIST SRM 2583 8 g
NIST2585 Organic contaminants in house dust NIST SRM 2585 10 g
NIST2681 Ashless blank filter NIST SRM 2681 set (10 filters)
NIST2692C Bituminous coal (sulfur, mercury, and chlorine) NIST SRM 2692c 50 g
NIST2702 Inorganics in marine sediment NIST SRM 2702 50 g
Today, NIST measurements support the smallest of technologies –nanoscale devices so tiny that tens of thousands can fit on the end of a single human hair – to the largest and most complex of human-made creations, from earthquake-resistant skyscrapers to wide-body jetliners to global communication networks.
Sigma-Aldrich® is proud to be the first licensed distributor of NIST Standard Reference Materials. Below you will find two tables containing environmental and food Standard Reference Materials® currently available from Sigma-Aldrich. The up-to-date list of all SRMs can be found on sigma-aldrich.com/nist
8
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9Feature ArticleStandards
Standard Reference Materials® for Food Analysis
Cat. No. Description Package SizeNIST1486 Bone meal NIST SRM 1486 50 gNIST1544 Fatty acids/cholesterol in frozen diet composite NIST SRM 1544 4 x 15 gNIST1546A Meat homogenate NIST SRM 1546a 4 x 85 gNIST1548A Typical diet NIST SRM 1548a set (2)NIST1549A Whole milk powder NIST SRM 1549a 5 x 10 gNIST1568B Rice flour NIST SRM 1568b 50 gNIST1570A Trace elements in spinach leaves NIST SRM 1570a 60 gNIST1573A Tomato leaves NIST SRM 1573a 50 gNIST17F Sucrose NIST SRM 17f, optical rotation 60 gNIST1849A Infant/adult nutritional formula NIST SRM 1849a 10 x 10 gNIST2383A Baby food composite NIST SRM 2383a 4 x 70 gNIST2387 Peanut butter NIST SRM 2387 3 x 170 gNIST2389A Amino acids in 0.1 mol/L hydrochloric acid NIST SRM 2389a 5 x 1.2 mLNIST3233 Fortified breakfast cereal NIST SRM 3233 60 g
NIST3234 Soy flour NIST SRM 3234 50 g
NIST3250 Serenoa repens (fruit) NIST SRM 3250 5 x 6 g
NIST3251 Serenoa repens extract NIST SRM 3251 5 x 1 mL
NIST3254 Camellia sinensis (green tea) leaves NIST SRM 3254 5 x 3 g
NIST3255 Camellia sinensis (green tea) extract NIST SRM 3255 5 x 1 g
NIST3256 Green tea-containing solid oral dosage form NIST SRM 3256 5 x 2.5 g
NIST3275 Omega-3 and Omega-6 fatty acids in fish oil NIST SRM 3275 2 x 3 x1.2 mL
NIST3278 Tocopherols in edible oils NIST SRM 3278 5 x 1 mL
NIST3280 Multivitamin/multielement tablets NIST SRM 3280 30 tablets x 5 bottles
NIST3283 Cranberry extract NIST SRM 3283 5 x 2.5 g
NIST3286 Organic acids calibration solution NIST SRM 3286 5 x 2 mL
Cat. No. Description Package SizeNIST2709A San Joaquin soil NIST SRM 2709a 50 g
NIST2710A Montana I soil NIST SRM 2710a 50 g
NIST2781 Domestic sludge NIST SRM 2781 40 g
NIST2783 Air particulate on filter media NIST SRM 2783 2+2 blank
NISTRM8529 IAEA-S-3 (sulfur isotopes in silver sulfide) NIST RM8529 0.5 g
NISTRM8536 GISP-Water NISTRM 8536 20 mL
NISTRM8537 SLAP-Water light stable isotopic standard NISTRM 8537 20 mL
NISTRM8541 USGS24 graphite (carbon isotopes in graphite) NIST RM 8541 0.8 g
NISTRM8542 Carbon isotopes in sucrose NIST RM 8542, IAEA-CH-6 sucrose 1 g
NISTRM8568 Nitrogen and oxygen isotopes in nitrate NIST RM 8568 0.9 g
NISTRM8569 Nitrogen and oxygen isotopes in nitrate NIST RM 8569 0.9 g
NISTRM8573 L-Glutamic acid NISTRM 8573, USGS40 1 g
9
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Analytix | 1: 2016 10
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Matrix Substances for MALDI-MSChoosing the right matrix for the analyte of interest is essential for any successful MALDI analysis. Sigma-Aldrich® offers the most comprehensive selection of pure and ultra-pure matrices for MALDI-MS, covering matrices suitable for many different analytes, such as proteins, peptides, polymers, lipids, oligonucleotides, and many more. Modern Ionic Liquid Matrices (ILMs) extend the unique properties of ionic liquids to MALDI-MS.
• High chemical purity to improve crystallization
• Low trace-metal content to minimize adduct formation and simplify the resulting MS spectrum
• Ultra-pure grades of the most popular matrix substances, with extremely strict specifications concerning purity, trace-metal content, appearance and solubility.
For a complete, up-to-date, and filterable product listing, please visit our Matrix Selection page at sigma-aldrich.com/maldimatrix
10
THE SIMPLE WAY TO ENSURE ACCURATE RESULTS, EVERY TIME.
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(ISO/IEC 17025)
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©2015 Sigma-Aldrich Co. LLC. All rights reserved. SIGMA-ALDRICH, is a trademarks of Sigma-Aldrich Co. LLC, registered in the US and other countries.
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• Matrices and Reagents
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11Feature ArticleStandards
Matthias Nold, Product Manager Analytical Standards
Sigma-Aldrich provides one of the most comprehensive offerings of analytical standards and certified reference materials (see also the TraceCERT® article on page 3 for the most recent certified reference materials) for pesticides, including metabolites. Under the renowned PESTANAL® brand, more than 1200 of the most widely used insecticides, herbicides, fungicides and other biocides are available as reference standards for food and environmental testing.
To serve the increasing demand for isotope labeled standards for isotope dilution methods, our competitively priced offering of these sometimes very difficult to find compounds is rapidly expanding. In Analytix 3/2015, which was issued in June of last year, we presented 26 new isotope labeled pesticide standards. In this issue, we can now proudly present the next 29 products in this range.
Find a complete and up-to-date listing at sigma-aldrich.com/pesticides
NEW Isotope Labeled Pesticide StandardsComplementing the Sigma-Aldrich® Comprehensive Range of Pesticide Standards
Cat. No. Description Package Size11355 Aldicarb-(N-methyl-13C,d3, carbamoyl-13C)
sulfone 5 mg
16202 Amitraz-(N-methyl-d3) 5 mg
16582 (±)-Bifenthrin-(biphenyl-2',3',4',5',6'-d5) 10 mg
49298 Carbendazim-(ring-4,5,6,7-d4) 5 mg
34517 Cyprodinil-(phenyl-13C6) 10 mg
74332 Diazinon-(diethyl-d10) 5 mg
74867 Dichlorvos-(dimethyl-d6) 10 mg
03627 Diquat dibromide-(ethylene-d4) 5 mg
34516 Folpet-d4 10 mg
Cat. No. Description Package Size74131 2-Imidazolidinethione-4,4,5,5-d4 10 mg
34523 Linuron-(methyl-d3, methoxy-d3) 10 mg
34541 Malathion diacid-(dimethyl-d6) 10 mg
34514 Malathion-(diethyl-d10) 10 mg
68405 MCPA-(methyl-d3) 10 mg
52485 Mepiquat-d16 chloride 5 mg
68458 Nitrofen-(nitrophenyl-d4) 10 mg
50636 Paraquat dichloride-(rings-d8) hydrate 5 mg
08979 trans-Permethrin-(phenoxy-d5) 5 mg
34515 Phenmedipham-(methoxy-d3) 10 mg
73879 Piperonylbutoxide-(butyl-d9) 10 mg
34536 Pirimiphos-methyl-(O,O-dimethyl-d6) 10 mg
68367 Prochloraz-(ethylene-d4) 10 mg
68326 Profenofos-(phenyl-d3) 10 mg
78937 Pyraclostrobin-(N-methoxy-d3) 5 mg
59603 Terbutryn-(S-methyl-d3) 10 mg
34572 Thiabendazole-(benzimidazole-3a,4,5,6,7,7a-13C6)
10 mg
30696 Thidiazuron-(phenyl-d5) 10 mg
74913 Trichlorfon-(dimethyl-d6) 10 mg
34538 Trifluralin-(dipropyl-d14) 10 mg
Table 1 New Isotope Labeled Pesticide Standards
11
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Analytix | 1: 2016 12
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sigma-aldrich.com/organiccrm
C
CH3 CH3
CH3 CH3
H3CCH3
CH3HO O
H3C CH3
O
HO
H3C
HO
Amarouciaxanthin A
C
CH3 CH3
CH3 CH3
H3CCH3
CH3HO O
H3C CH3
OH
HO
CH3HO
Isofucoxanthinol
C
CH3 CH3
CH3 CH3
H3CCH3
CH3HO O
H3C CH3
OH
HOO
H3CFucoxanthinol
Matthias Nold, Product Manager Analytical Standards
In a previous issue of Analytix (5/2015), we published an article that discussed the relevance of distinguishing between different isomers of the carotenoid astaxanthin, namely the 9-cis, 13-cis and all-trans isomers (the issue is downloadable at sigma-aldrich.com/analytix).
Generally, carotenoids and their presence in food are receiving increased attention because of their beneficial effects as antioxidants.
Therefore, Sigma-Aldrich® is rapidly increasing its range of analytical standards for carotenoids. The latest product additions are listed below. For the complete offering of carotenoid standards, please visit sigma-aldrich.com/carotenoids
Cat. No. Description Package Size54758 Amarouciaxanthin A 1 mg72723 Fucoxanthinol 1 mg74132 Isofucoxanthinol 1 mg72994 Neoxanthin 1 mg
Table 1 New Carotenoid Standards
Neoxanthin
C
CH3 CH3
CH3
CH3CH3
H3C
HO
OHH
CH3 H3C CH3
O
H3C OH
Neoxanthin is a major carotenoid contained in spinach and other leafy vegetables.
sigma-aldrich.com/carotenoids 12
Neoxanthin and Other CarotenoidsNew Analytical Standards for Food Testing
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13Feature ArticleStandards
NEW Certified Reference Materials for ISO Method 17943
Cory E. Muraco, R&D Scientist at Supelco
Volatile organic compounds (VOCs) are commonly used in the manufacturing processes of several everyday items including paints, petroleum products, refrigerants, pharmaceuticals, and dry-cleaning agents. VOCs are also employed by nature to act as chemical messengers between plants and by insects and animals as a deterrent to prevent predation. However, VOCs can be toxic to human health if one is exposed continuously to VOCs. This problem is most prevalent from off-gassing of building materials, thus creating indoor air concentrations of VOCs that are above permissible limits. VOCs are harmful to the environment; one way for them to get into the environment is from aqueous runoff from factories, waste
disposal/recycling facilities, and municipalities mixing with natural water sources.
The International Organization for Standardization (ISO) has developed a new method for the determination of VOCs in water by headspace SPME/GC-MS. This method measures the concentrations of over 60 VOCs in a water sample. Certified reference materials (CRMs) are required to calibrate the method. Supelco®, an ISO/IEC 17025, Guide 34 doubly-accredited facility, has developed three CRMs that cover the entire scope of ISO 17943. Table 1 lists the components of these mixes. For more information about CRMs, please visit sigma-aldrich.com/standards
13
Cat. No. Description Composition ConcentrationPackage
Size44923-U ISO 17943 Odor
Compounds Mix(+/-)-Geosmin Methylisoborneol
2-Ethyl-4-methyl-1,3-dioxolane 2-Ethyl-5,5-dimethyl-1,3-dioxane
200 µg/mL in methanol 1 x 1 mL
44926-U ISO 17943 VOC 57 Compounds Mix tert-Amyl methyl ether
Benzene
Bromobenzene
Bromochloromethane
Bromodichloromethane
Bromoform
Butylbenzene
sec-Butylbenzene
tert-Butylbenzene
tert-Butyl ethyl ether
Carbon tetrachloride
Chlorobenzene
Chloroform
2-Chlorotoluene
4-Chlorotoluene
Cumene
Dibromochloromethane
Dibromomethane
1,2-Dibromo-3-chloropropane
1,2-Dibromoethane
1,2-Dichlorobenzene
1,3-Dichlorobenzene
1,4-Dichlorobenzene
1,1-Dichloroethane
1,2-Dichloroethane
1,1-Dichloroethene
trans-1,2-Dichloroethene
cis-1,2-Dichloroethene
Dichloromethane
1,2-Dichloropropane
1,3-Dichloropropane
2,2-Dichloropropane
1,1-Dichloropropene
cis-1,3-Dichloropropene
trans-1,3-Dichloropropene
Ethylbenzene
Hexachlorobutadiene
p-Isopropyltoluene
200 µg/mL in methanol
Methyl tert-butyl ether
Naphthalene
n-Propylbenzene
Styrene
1,1,1,2-Tetrachloroethane
1,1,2,2-Tetrachloroethane
Tetrachloroethene
Toluene
1,2,3-Trichlorobenzene
1,2,4-Trichlorobenzene
1,1,1-Trichloroethane
1,1,2-Trichloroethane
Trichloroethylene
1,2,3-Trichloropropane
1,3,5-Trimethylbenzene
1,2,4-Trimethylbenzene
m-Xylene
o-Xylene
p-Xylene
1 x 1 mL
48625 Vinyl chloride Vinyl chloride 200 µg/mL in methanol 1 x 1 mL
Table 1 New ISO 17943 Method Certified Reference Materials
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Analytix | 1: 2016 14
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Products from Jaytee® Now at Sigma-Aldrich®Kromega Range of Qualification Standards
Magdalena Ulman, Product Manager Analytical Reagents
Jaytee is well respected among the UK’s largest pharmaceutical and chemical companies as a quality lead supplier and service provider. The current product range covers a variety of HPLC (or UHPLC) CRMs suitable for calibrating systems with any style of UV detection and a range of UV/Visible Spectroscopy CRMs, which meet the European Pharmacopeia’s requirements for the calibration of UV/Vis spectrophotometers. Future additions to the range will include GC FID and other HPLC detectors.
Certified Qualification Standards are designed to support your work:
• Calibration/validation activities built on a solid foundation
• Only variable in the qualification process is the instrument
• Standards developed for use in any laboratory, regardless of the regulator, and as relevant to a pharmaceutical company as to a contract lab working to ISO 17025
• Standards shipped in flame-sealed ampoules individually seated in custom-made boxes increase the shelf life and prevent contamination
• Cost for an organization is minimal, as compared with developing a custom solution. For companies complying to any form of GxP regulation, there is a stated need to qualify equipment that generates data; “out of the box” solution meets that requirement
• Easy, cost-effective means of achieving conformance, since all regulators require that qualification is traceable
• Traceable instrument qualification adds confidence to all data generated; audit trail backed up by the independent verification by UKAS to ISO Guide 34
At Sigma-Aldrich the following CRMs are now available:
Kromega CRMs for HPLC:
Cat. No. Description Z803898 HPLC Autosampler
Z804002 UV Absorbance Linearity
Z804126 UV Low Wavelength
Z804223 UV Multi Wavelength
Z804339 HPLC Qualification Kit
Kromega CRMs for UV/Visible Spectrophotometers:
Cat. No. Description Z804452 UV Photometric Accuracy
Z804568 UV Resolution (EP)
Z804665 UV Stray Light (EP)
Z804789 UV Spec Qualification Kit
Please, visit our website at sigma-aldrich.com/jaytee to get more information.
14
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15Feature ArticleStandards
New Products from Glass Expansion® Now Available at Sigma-Aldrich®
Glass Expansion is combining forces with Sigma-Aldrich to bring you products that demonstrate excellent product quality and proven outstanding performance in the area of ICP and ICP-MS.
Please visit our website at sigma-aldrich.com/gx to get more information regarding our new, continually improving product line of accessories and consumables for ICP and ICP-MS such as nebulizers, spray chambers, torches and other parts.
UV-Vis Optical Components Line from Hellma®Portfolio of our Hellma products includes:
• Cells for absorption, fluorescence and special application measurements
• UV-Vis calibration standards
• Cleaning concentrate for cells and optical components
• Accessories
Please, visit our website at sigma-aldrich.com/hellma to get more information.
15
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Analytix | 1: 2016 16
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ULTRA100 Certified Low Level TOC VialsFrom Dual Accredited Producer Altus Science
Jens Boertz, Product Manager Analytical Reagents
Lisa Fitzpatrick, Tactical Marketing Manager
Total organic carbon (TOC) can be used as a non-specific indicator of water quality or cleanliness of pharmaceutical manufacturing equipment. Meticulously cleaned vials are essential in supporting these measurements. Individual certificates of conformance are included with each case of vials.
About Altus ScienceAltus Science is a Certified Reference Material (CRM) provider, focusing on Total Organic Carbon (TOC) and Conductivity CRMs. Altus Science provides Calibration, Validation and Consumables for all makes of TOC analyzers.
Altus Science recognizes the importance of high quality CRMs. The facility is home to a range of analytical instruments used for verification purposes
Cat. No. Description Package SizeULTRA06 Box of 6 x 40 mL Certified Clean Borosilicate Glass Vials with 24 mm Cap and Silicone PTFE Lined Septa. Case
includes individual certificate. Certified vials have <0.010 mg/L C from TOC. All 6 vials also include dust caps.6 EA
ULTRA100 Box of 100 x 40 mL Certified Clean Borosilicate Glass Vials with 24 mm Cap and Silicone PTFE Lined Septa. Case includes individual certificate. Certified vials have <0.010 mg/L C from TOC. All 100 vials also include dust caps.
100 EA
A-2025-040 ISO 17025 & ISO Guide 34 CRM – USP TOC System Suitability Set. Set includes 4 x 40 mL vials – 2 USP reagent water. 1 of 0.500 mg/L C USP Sucrose & 1 x 0.500 mg/L from USP 1,4-Benzoquinone – all CRMs are phosphoric acid stabilized – kit comes with individual certificate of analysis for each CRM.
1 EA
Altus Science began trading in 2012 and was successfully assessed by UKAS and audited to both ISO 17025 and ISO Guide 34 in July 2013. The culture of quality is a fundamental foundation of Altus Science’s business.
Based in Vanguard House in Sci-Tech Daresbury, UK, Altus Science operates a tightly controlled manufacturing facility.
16
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17Feature ArticleLabware
Timestrip® The Smart Way to Measure Time and Temperature
Daniel Weibel, Product Manager Analytical Reagents
In 2015 we introduced two ranges of analog indicators, Timestrip, which indicates the passing of time, and Timestrip PLUS, which indicates time spent above a critical temperature. They have been so successful that we have added six new variants to the range. In this sixth article (see: Analytix 1-5/2015), we introduce the new variants.
Get Control of Time – activate a Timestrip to track time. A fail-safe, cost-effective reminder or when your product has expired or you need to carry out a task. Simply activate and watch the colored liquid move through the viewing window to indicate passing time.
Three new shorter-duration Timestrip variants are now available to order: 1 hour, 12 hours and 7 days (Figure 1). Potential uses include tracking diagnostic tests, testing kits, disinfecting periods and medical devices. The seven Timestrip variants you can order now provide a monitoring solution for fifteen different time periods (including the interval markers):
• ½, 1, 3, 6, 12 hours
• 1, 3, 7 days
• ½, 1, 2, 3, 6, 9, 12 months
Three new temperature indicators are now available to order.
Some cold chain products can tolerate breaches longer than 8 hours, so you can now order the Timestrip PLUS 8 °C with either an 8 hour or a 48 hour window.
To meet increasing demand by the food testing and premium food shipping sectors, Timestrip has created two new products. Once activated, each one monitors temperature and only indicates if cumulative breaches of 5 °C (Food) or 3 °C (Seafood) have reached a minimum of 2 hours, and records further breaches up to a maximum of 4 hours.
Cat. No. Description 89148 NEW Timestrip 1 hour
80956 NEW Timestrip 12 hours
88790 NEW Timestrip 7 days
80826 NEW Timestrip Plus 8 °C 48 hours
07475 NEW Timestrip Food
06732 NEW Timestrip Seafood
93064 Timestrip 1 month
07603 Timestrip 3 months
06797 Timestrip 6 months
74831 Timestrip 12 months
03849 Timestrip 3 months, key chain
06929 Timestrip 12 months, key chain
06693 Timestrip Plus -20 °C
92210 Timestrip Plus 0 °C
08168 Timestrip Plus 8 °C
92451 Timestrip Plus 25 °C
80474 Timestrip Plus 30 °C
80476 Timestrip Plus Duo 10 °C and 34 °C
Table 1 Timestrip Indicators are Available in Package Sizes of 10 EA, 100 EA and 500 EA
1 hour 12 hours 7 daysFigure 1 Three New Timestrip Time Indicators with Shorter-Duration Window
Get Control of Temperature – activate a Timestrip PLUS and check temperature abuse of your product. Simply squeeze the button to activate, chill to the required temperature for one hour, and use. Color will appear in the viewing window to show how long temperatures have been above the critical temperature.
3 °C threshold 5 °C threshold
Figure 3 Timestrip Food and Seafood for Use in F&B Markets
Figure 2 Timestrip PLUS 8 °C Now Available with Two Different Time WindowsLearn more at sigma-aldrich.com/timestrip or contact us at [email protected]
17
Current NEW (activation button on the back)
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Analytix | 1: 2016 18
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Figure 1 Extracted Ion Chromatograms (EIC) of fructose-1,6- and fructose-2,6-bis-phosphate Separated on a Supelco® Ascentis® Express C18, 2.1x50 mm column (2.7 µm). The Mobile Phases are 10 mM tributylammonium acetate (pH 5) and methanol (Gradient: 0 min 95% aqueous, 1.2 min 95%, 10 min 65%, 20 min 65% @ 0.3 ml/min). Fructose-2,6-bis-phosphate was not Detected Without IPC Reagent.
Rudolf Köhling, Sr. Scientist
Eric Allenspach, R&D Technician
Sugars play a key role in cell processes and in all higher organisms. Starting with DNA and protein biosynthesis, they also serve as energy sources or can be found as second messengers in signal transduction and cell regulation processes. Sugars and their metabolites, e.g., acids, phosphorylated sugars, etc., represent a major group of compounds in metabolic pathways. Unfortunately, most of them are highly polar and non-UV absorbing.
The separation of highly polar compounds by HPLC is challenging, especially for reversed-phase mobile phase compositions. Often ion-exchange, ion chromatography or capillary electrophoresis are better alternatives, since hyphenation with mass spectrometry has restrictions caused by column bleeding, incompatible buffers or modified ion sources [1–3].
Recent publications on sugars and their related metabolites describe HILIC- or ion-pair chromatography (IPC)-based methods for LC-MS. In the following example, IPC is applied for the separation of phosphorylated sugars using dihexylammonium and tributylammonium acetate as IPC reagents [2,4]. Both reagents have the same molecular weight but they differ in vapor pressure and basicity, which we found is crucial in the detection of some analytes, e.g., fructose-2,6-bis-phosphate. We found a better sensitivity and selectivity for the separation of fructose-1,6- and fructose-2,6-bis-phosphate with tributylammonium acetate buffer according to [2]. The higher basicity of tributylamine enhances the detection of [M-H] ions. Additionally, a higher vapor pressure reduces the formation of charged particles in a CAD detector and lowers the background noise and baseline.
Trying different IPC reagents during method development, e.g., dihexylamine, tributylamine, and dibutylamine, can improve the separation. In some cases IPC can be the best option to solve a chromatographic problem even for LC-MS [5].
Ion-Pair Chromatography of Phosphorylated Sugar Metabolites
Cat. No. Description53822-U Ascentis® Express C18, 2.7 Micron HPLC Column73345 Dibutylamine acetate solution, 0.5M, for ion pair
chromatography, concentrate, ampoule92467 Dihexylamine acetate solution, 0.5M, for ion pair
chromatography, concentrate, ampoule89789 Dipropylamine acetate solution, 0.5M, for ion pair
chromatography, concentrate, ampoule49540 Heptafluorobutyric acid solution, 0.5M, for ion pair
chromatography90781 Tributylamine, puriss. plus, >= 99.5 % GC
References:[1] Soga T. et al, Anal. Chem. 2002, 74, 2233-2239.[2] Arrivault S. et al, The Plant Journal 2009, 59, 826–839.[3] Lunn J.E. et al, Biochem. J. 2006, 397, 139–148.[4] Uematsu K. et al, J. Exp. Bot. 2012, 1-9.[5] Köhling R. Separation and Detection of Phosphorylated Metabolites,
Poster 47, Montreux LC-MS Meeting, 2012.
Sigma-Aldrich® offers an outstanding range of tailor-made ion pair reagents for anionic (quaternary ammonium and phosphonium salts) and cationic (alkanesulfonates) determination. All mobile phase additives are subject to rigorous testing with special emphasis on the requirements of modern reversed phase HPLC. Learn more at sigma-aldrich.com/ipc
18
11.0
83
Inte
nsity
0.0
1.0x105
2.0x105
3.0x105
4.0x105
5.0x105
6.0x105
7.0x105
8.0x105
9.0x105
1.0x106
1.1x106
1.2x106
1.3x106
Minutes0.00 2.00 4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00
10.9
31
Inte
nsity
0
100000
200000
300000
400000
500000
600000
700000
Minutes0.00 2.00 4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00
Fructose-2,6-bis-phosphate
Fructose-1,6-bis-phosphate
11.0
83
Inte
nsity
0.0
1.0x105
2.0x105
3.0x105
4.0x105
5.0x105
6.0x105
7.0x105
8.0x105
9.0x105
1.0x106
1.1x106
1.2x106
1.3x106
Minutes0.00 2.00 4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00
10.9
31
Inte
nsity
0
100000
200000
300000
400000
500000
600000
700000
Minutes0.00 2.00 4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00
Fructose-2,6-bis-phosphate
Fructose-1,6-bis-phosphate
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19Feature ArticleChromatography
New TLC Staining Solution for Boronic Acids Curcumin solution 28982 effectively stains various types of boron-containing species, such as:
• Free boronic acids
• Boronic acid pinacol esters
• Potassium trifluoroborate saltsFor rapid monitoring of your Suzuki-Miyaura cross-coupling, or any other organic reaction involving boronic acids and related derivatives, try curcumin solution 28982.
For more information on TLC derivatization, visit sigma-aldrich.com/derivatization
[1] Lawrence, K.; Flower, S. E.; Kociok-Kohn, G.; Frost, C. G.; James, T. D., A simple and effective colorimetric technique for the detection of boronic acids and their derivatives. Anal. Methods 2012, 4, 2215–2217.
1 691615 (+)-Vinylboronic acid pinanediol ester
2 674710 3-Methoxy-1-propyn-1-ylboronic acid pinacol ester
3 346225 (2-Methylpropyl)-boronic acid
4 683590 Potassium trans-3-methoxy- 1-propenyltri-fluoroborate
1 2 3
A Safer Way to Open Glass AmpoulesSnapITs are easy-to-use, multi-use ampoule openers that prevent the possibility of injury sometimes seen when ampoules are opened by hand.
1 INSERT the ampoule lid into your multi-use SnapIT2 SNAP open the ampoule3 EJECT the ampoule lid directly into a sharps containerSnapIT ampoule openers help you move toward a safer workplace. They are available in two slimline cylindrical designs: regular and large.
Cat. No. Description Ampoule Size Compatibility94791 Ampoule opener – Regular 1–2 ml, 5–10 ml,
10 –15 ml
43917 Ampoule opener – Large 5–10 ml, 10 –15 ml, 20–25 ml
19
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Date: 02/2016Lit. Code: RXI
