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Issue32011AnalytixWaterDeterminationinMilkandMilkProductsWaterDeterminationinDairyProductsNewUHPLCSolventsSalmonellaDetectionNewDerivatizationReagentsNewSolventsforGC-HeadspaceCertifiedReferenceMaterialsReferenceMaterialforHerbalMedicine2EditorialExpandedQualitytoMeetYourAnalyticalNeeds–IntroducingCerilliantandResourceTechnologyCorporation(RTC),thetwonewestadditionstoSigma-AldrichDearColleague,Inoureffortstobringyouthehighestqualityandbestofferingofanalyticalproducts,Sigma-Aldrichwouldliketowelcomeourtwonewestfamilymembers,CerilliantCorporationofRoundRock,TexasandRTCofLaramie,Wyoming.
TheextensivecapabilitiesofthesetwocompaniescomplementSigma-Aldrich'sexistingFlukaandSupelcoanalyticalbrands.
Cerilliant'squalitycredentialsincludeaccred-itationtoISOGuide34andISO/IEC17025,certi-ficationtoISO9001:2008andincorporationofcGMPandGLPrequirementsintotheireverydayactivities.
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Cerilliantoffersover2,800productsandmorethan30yearsofexpertiseinthedesign,development,synthesis,characterisationandpackagingofanalyticalstandards,calibra-tors,controlsandcertifiedreferencematerialsforthepharmaceutical,clinicaldiagnostics,forensicandclinicaltoxicology,nutraceuticalandenvironmentalmarkets.
RTCisapremiummanufacturerofCertifiedReferenceMaterials(CRMs),QualityControl(QC)Samples,andProficiencyTesting(PT)Sampleswithmorethan20yearsofexperienceandastrongexpertiseintheenvironmentalaswellasinthepharmaceuticalsector.
RTCwasoneoftheoriginalProficiencyTestprovidersrecognisedbytheUSEPA.
ItsqualitysystemsincludeISO/IEC17025,ISOGuide34(CRMs),ISO/IEC17043(PT)andISO9001:2000.
AddtheoutstandingexpertiseofCerilliantandRTCtotheover40yearsofexperienceatSupelcoand60yearsatFlukaandyouhaveanunmatchedamountofknowledgeandproductsavailableforyourlaboratoryneeds.
Thesecompa-nieswillcombinetheirtalentsandcapabilitieswiththoseofSigma-AldrichtocreatevisionaryapproachestosupplytheanalyticalindustrywithacontinuallyexpandinglistofnewproductsthatmeetthemostrigorousqualityrequirementsincludingcGMP,GLPandISOrequirements.
CurrentlytheproductsofCerilliantandRTCareonlyavail-ablethroughCerilliantandRTCthemselvesoroneoftheirdistributors.
Pleasecontactthemdirectlyorvisitwww.
cerilliant.
comorwww.
rt-corp.
comtoreviewproducts,toaskaquestionortoplaceanorder.
Kindregards,Dr.
IngoHaagDirectorMarketingIngo.
Haag@sial.
comDr.
IngoHaagDirectorMarketingAnalytixispublishedfivetimesperyearbySigma-AldrichChemieGmbH,MarComEurope,Industriestrasse25,CH-9471BuchsSG,SwitzerlandPublisher:Sigma-AldrichMarketingCommunicationsEuropePublicationdirector:IngoHaag,PhDEditor:DanielVoglersigma-aldrich.
com/analytix33TableofContentssigma-aldrich.
com/analytixStandards17DAIH-andDNPH-AldehydeandKetoneStandards19NewAnalyticalStandardsfortheAnalysisofHerbalMedicinalProducts21NewTraceCERTOrganicCertifiedReferenceMaterialsTitration22VolumetricTitrationVOLPACSolutionContainerswithnewadapterFeatureArticle4WaterDeterminationinMilkandMilkProductsKarlFischerTitrationwithHYDRANALReagentsMicrobiology8Salmonella'sTricksandtheirDetectionDerivatization11NewDerivatizationReagentsChromatography12UHPLC–State-of-the-ArtinChromatographySigma-AldrichintroducesLC-MSUltraCHROMASOLV16NewHeadspaceGradeSolventsNewProductCorner15NewSELECTOPHOREIonophoreswithImprovedProperties4sigma-aldrich.
com/hydranalFeatureArticleWaterDeterminationinMilkandMilkProductsKarlFischerTitrationwithHYDRANALReagentsIntheproductionofmilkanddairyproducts,watercontentplaysanimportantrole,technologicallyaswellaseconomically.
Therefore,nationalandinternationallawsandagreementsprotectandregulatethedefinitionofproductsandtheproductionprocessesindairytechnology.
Determiningthewatercontentinmilkandmilkpro-ductscanbeeasilyachievedwithKarlFischer(KF)titration.
Wholemilkisacolloidalsystemcomposedofacontinuousaqueousphaseinwhichlactose,wheyproteins,andmineralsaredissolved.
Thedispersedphaseconsistsofcaseinmicellesandfatglobules.
Wholecow'smilktypicallycontains90g/kgofnon-fatsolidsandbetween35to40g/kgoffat.
Boththefatglobulesandthecaseinmicellescontributetothewhitenessofmilkbylightscattering.
Creamcanbeconsi-deredaconcentrateddispersionoffatglobules,whileskimmilkcontainsresidualmilkfatoflessthan0.
1%.
ProductionofMilkandMilkproductsAnimportantstepintheindustrialproductionofmilkproducts(Figure1)istheseparationofmilkintocreamandskimmilk.
Creamcanbeconsideredasthefatpartofthemilk,whileskimmilkispracticallyfat-free,containingwater,milkproteins,andlactose.
Butterismadefromcream,whereasbuttermilkistheremainingliquidfromthisprocess.
Rawmilk(orcreamandskimmilkcombinedasingredients)isthebasicmaterialformanyothermilkproducts,suchascheese,milkpowder,condensedmilk,andfermentedmilkproducts.
DrinkingMilk–TreatmentsandclassificationTheEuropeanCommissiondefinesdifferenttypesofconsumermilks:Rawmilkhasnotbeenheatedabove40°CWholemilkhasbeenheat-treated(pasteurizedorsterilized)Pasteurizationisusedtodestroyallpathogenicmicroorganismsinmilk.
Theso-calledcontinuoushigh-temperatureshort-time(HTST)procedureprescribesarapidheatingofthemilktotemperaturesfrom71-74°C,andholdingtheproductatthistemperaturefor15to20seconds.
SterilizationofmilkcanbeachievedbyUltrahighTemperatureheating(UHT).
ThecharacteristictemperaturerangeforUHTheatingis135-150°Cwithholdingtimesofafewseconds.
ThegoalofUHTprocessingistoaccomplishasterileproductstorableatambienttemperature.
Thisheattreatmentdestroysallmicroorganismsandtheproductisthenpackagedasepticallyintosterile,hermeticallysealedpackages.
AndreaFelgner,ProductManagerAnalyticalReagentsandrea.
felgner@sial.
comThomasWendt,HYDRANALTechnicalServicethomas.
wendt@sial.
comFigure1ProductionstepsofmilkandmilkproductsDrinkingMilkButtermilkButterCheeseMilkPowderCondensedMilkWheyMilkProteinsSkimMilkCream(Fat)RawMilkDrinkingMilkLactoseFermented/CulturedMilkProducts5sigma-aldrich.
com/hydranalFeatureArticle(continuedonpage6)EURegulationUSARegulationNon-standardizedwholemilkUnchangedfatcontent,notlessthan3.
5%WholemilkMinimumfatcontentof3.
25%Fat-adjustedwholemilkModifiedfatcontent,notlessthan3.
5%(actualcontentindicatedonthepackage)Reduced-fatmilkFatcontentof2%PartiallyskimmedmilkAdjustedfatcontentof1.
5%-1.
8%Low-fatmilkFatcontentof1%SkimmilkFatcontentofmaximum0.
5%SkimmilkFatcontentmaximum0.
5%(maybecalled"fatfree")Table2ClassificationofDrinkingMilk(EUandUSA)ProductMilkfatcontentWatercontentMilkproteininmilksolids-not-fatCreampowderMin.
42%m/mMax.
5%m/mMin.
34%m/mWholemilkpowderMin.
26%m/mMax.
42%m/mPartlyskimmedmilkpowderMin.
1.
5%m/mMax.
26%m/mSkimmedmilkpowderMax.
1.
5%m/mTable3CompositionofmilkpowdersOtherMilkProductsEvaporated/CondensedMilkisproducedthroughthecon-centrationanddryingofmilk.
Theseprocessingstepsleadtoproductswithasmallervolumeandalongershelflife.
Tofurtherenhancetheshelflifeoftheseproducts,heattreat-mentforsterilizationcanbeapplied.
Thepartialremovalofwaterfrommilkorcreamleadstoproductionofmilkpowderorcreampowder.
Thefatand/orproteincontentofthemilkorcreammaybeadjustedbytheadditionand/orwithdrawalofmilkconstituents.
Theaccuratecontrolandadjustmentofaprecisevalueofwatercontentisespeciallysignificantformilkpowders(Table3).
ApplicationWaterdeterminationincoffeecream,quark(cheese),milk,milkpowder,yoghurtMilkconsistsmainlyofwater;therefore,itswatercontentdeterminationisstraightforward.
AlloftheseproductsreleasetheirwatereasilyintheworkingmediumoftheKFtitration;thedeterminationcanbecarriedoutwithclassicalKFreagents.
However,itisveryoftennecessarytotakeintoaccounttheinhomogeneouswaterdistributionorsepara-tionofcomponentsduringstorage.
Ahomogenizationbeforetakingthesampleisrecommended,especiallyforquarkandyoghurt.
Fortitrationofmilkpowder,aheatingofthereagentsto50°Cmaybebeneficial.
Sincemilkpowderatthistemperaturereleasesitswatercontentonlyslowly,thedeterminationcanbeacceleratedathighertempera-tures.
Milkpowderwithespeciallyhighfatcontentmayneedtheadditionofchloroformtotheworkingmediumtoimprovethesolubilityofthesample.
CoulometricKFtitra-tionisnotrecommendedforthesesamples.
Samplesizesanddosage:Coffeecream0.
1g/syringewithneedleMilk0.
05g/syringewithneedleMilkpowder1.
0g/powderfunnelQuark0.
1g/syringewithoutneedleYoghurt0.
1g/syringewithoutneedleVolumetricKFtechniqueReagentOne-componenttechniqueTitratingagentHYDRANAL-Composite5WorkingmediumHYDRANAL-MethanolRapidorHYDRANAL-MethanoldryReagentTwo-componenttechniqueTitratingagentHYDRANAL-Titrant5WorkingmediumHYDRANAL-SolventProductWaterProteinFatCarbohydratesOrganicacidsMineralsWholemilk87.
7%3.
3%3.
6%4.
6%0.
2%0.
7%Fat-reducedmilk89.
6%3.
4%1.
6%4.
6%0.
2%0.
7%Skimmilk90.
9%3.
5%0.
1%4.
8%0.
2%0.
8%Buttermilk91.
2%3.
5%0.
5%4.
0%0.
8%0.
8%Whey(sweet)93.
6%0.
8%0.
2%4.
7%0.
3%0.
6%Condensedmilk74.
7%6.
5%7.
6%9.
2%0.
3%1.
5%Coffeecream81.
7%3.
1%10.
5%4.
1%-0.
6%Table1Nutritionalcompositionofmilkproducts6sigma-aldrich.
com/hydranalFeatureArticleApplicationWaterdeterminationincheeseCheesedoesnotdissolveinmethanolandthereforedoesnotreleaseitswatercontentinclassicalKFsolvents.
Theadditionofformamidetotheworkingmediumasasolubil-izerisnecessary;carryingoutthetitrationatelevatedtem-peraturesisalsorecommended.
Thesampleshouldbefinelygratedorcutintosmallpieces;thistypeofsamplewillgiveaturbidsolutionwiththeworkingmediumafterstirringfor5-10minutes;thefollowingtitrationshouldtakeabout2-3minutes(samplesize0.
2g/powderfunnel).
CoulometricKFtitrationisnotrecommendedforthissample.
VolumetricKFtechniqueReagentOne-componenttechniqueTitratingagentHYDRANAL-Composite5WorkingmediumHYDRANAL-Methanoldry/RapidandHYDRANAL-Formamidedry1:1Two-componenttechniqueTitratingagentHYDRANAL-Titrant5WorkingmediumHYDRANAL-SolventandHYDRANAL-Formamidedry1:1ApplicationWaterdeterminationinicecreamThesampleshouldbemeltedandcarefullyhomogenizedbeforetheanalysis.
Toimprovethedissolutionofthefatcontent,thetitrationshouldbecarriedoutinHYDRANAL-LipoSolverCM,whichcontainschloroform(samplesize0.
05g/syringewithoutneedle).
CoulometricKFtitrationisnotrecommendedforthissample.
VolumetricKFtechniqueReagentOne-componenttechniqueTitratingagentHYDRANAL-Composite5WorkingmediumHYDRANAL-LipoSolverCM(orHYDRANAL-Methanoldry/RapidandHYDRANAL-Chloroform1:1)Two-componenttechniqueTitratingagentHYDRANAL-Titrant5WorkingmediumHYDRANAL-SolventCM(orHYDRANAL-SolventandHYDRANAL-Chloroform2:1)ApplicationWaterdeterminationinwheyfatemulsionThisproductmaycoattheelectrodesinthetitrationcell.
Fadingend-pointsanderroneouslyhighresultsaretheconsequencesofthisinterference.
Theadditionofform-amidetotheworkingmediumcanpreventthisinterference,whileadditionofchloroformisnecessarytodissolvethefatofthesample(samplesize0.
1g/syringewithoutneedle).
CoulometricKFtitrationisnotrecommendedforthissample.
VolumetricKFtechniqueReagentOne-componenttechniqueTitratingagentHYDRANAL-Composite5WorkingmediumHYDRANAL-MethanoldryandHYDRANAL-ChloroformandHYDRANAL-Formamidedry1:1:1Two-componenttechniqueTitratingagentHYDRANAL-Titrant5WorkingmediumHYDRANAL-SolventandHYDRANAL-ChloroformandHYDRANAL-Formamidedry2:1:17sigma-aldrich.
com/hydranalFeatureArticleApplicationWaterdeterminationinwheypowderInourinvestigations,thissampleshowedasmallsidereactionwithiodine.
ThesereactionsareoftenpH-dependent;HYDRANAL-BufferBaseoraworkingmediumcontainingaportionofsalicylicacidhelpstosuppressthissecondaryre-action.
Atitrationatelevatedtemperaturesenhancesthesidereactionandisthereforenotrecommended.
Todissolvethehighlactosecontentcontainedinthesample,theadditionofformamideisalsonecessary(samplesize0.
5g/powderfunnel).
CoulometricKFtitrationisnotrecommendedforthissample.
VolumetricKFtechniqueReagentOne-componenttechniqueTitratingagentHYDRANAL-Composite5WorkingmediumHYDRANAL-BufferBase(orHYDRANAL-Methanoldry/Rapidand5gHYDRANAL-Salicylicacid)andHYDRANAL-Formamidedry2:1Two-componenttechniqueTitratingagentHYDRANAL-Titrant5WorkingmediumHYDRANAL-SolventandHYDRANAL-Formamidedry2:1plus5gHYDRANAL-SalicylicacidApplicationreports(availableuponrequestfromhydranal@sial.
com):L074Quark(cheese)L077WheyfatemulsionL081Milkpowder(wholemilk)L082Milkpowder(skimmedmilk)L085MilkL095CheeseL097YoghurtL222CoffeecreamL493Whey(powdered)L523IcecreamCat.
No.
DescriptionVolumetricone-componentreagents34805HYDRANAL-Composite534806HYDRANAL-Composite234827HYDRANAL-Composite134741HYDRANAL-Methanoldry37817HYDRANAL-MethanolRapid34734HYDRANAL-CompoSolverE37855HYDRANAL-LipoSolverCMVolumetrictwo-componentreagents34732HYDRANAL-Titrant5E34723HYDRANAL-Titrant2E34801HYDRANAL-Titrant534811HYDRANAL-Titrant234730HYDRANAL-SolventE34800HYDRANAL-Solvent34812HYDRANAL-SolventCMAuxiliaryReagents(Solubilizers)37863HYDRANAL-Chloroform34724HYDRANAL-Formamidedry37865HYDRANAL-Salicylicacid34804HYDRANAL-BufferAcid37859HYDRANAL-BufferBaseWaterstandardsfortiterdetermination34849HYDRANAL-WaterStandard10.
034696HYDRANAL-StandardsodiumtartratedihydrateTable4SelectedFlukabrandHYDRANALKarlFischerreagentsReferences[1]Jost,R.
MilkandDairyProducts.
Ullmann'sEncyclopediaofIndustrialChemistry,2007.
[2]LebensmitteltabellefürdiePraxis.
Editor:DeutscheForschungsanstaltfürLebensmittelchemie,GarchingbeiMünchen.
WissenschaftlicheVerlagsgesellschaftStuttgart,2009.
[3]CodexAlimentarius"Codexstandardformilkpowdersandcreampowder".
CODEXSTAN207-1999.
FAO/WHO.
Sigma-Aldrichoffersover650applicationreports.
AfulllistofthesereportsandallHYDRANALproductscanbefoundonourwebsitesigma-aldrich.
com/hydranalToobtainanapplicationreport,pleasecontactoneofourHYDRANALlaboratories:EuropeandGlobalMarketMr.
ThomasWendtTechnicalServiceHYDRANALD-30926Seelze,GermanyTel.
:+49(0)51378238-353Fax:+49(0)51378238-698E-Mail:hydranal@sial.
comUSAandCanadaMr.
DougClarkHYDRANALTechnicalCenterSt.
LouisMO63103,USATollfree:+1800493-7262(USAandCanada)Fax:+1314286-6699E-Mail:hydranal@sial.
com8sigma-aldrich.
com/salmonellaMicrobiologyThemediausedcurrentlyforthedifferentiationandidenti-ficationofSalmonellaarestillbasedonthedetectionofcarbohydratefermentationindicatedbyapHindicator(seeTable2forcarbohydratefermentationability),thedetec-tionofproteolyticactivity,hydrogensulphideproductionandselectivity.
Mostmodernmediaalsocombineaspectsofthisdetectionsystemtomakethemediamorereliable.
AlistingofthemostcommonselectiveanddifferentialmediaappearsinTable3.
Foratypicalmicrobiologicalcontrolprocedure,pleaseseetheISOmethodillustratedinFigure2.
Inaddition,Sigma-Aldrich'sinnovativetechnologyhasdevelopedalineofchromogenicmediaproductswhichmakeidentificationevenmorereliableandfasterastheydetectacharacteristicenzymeofSalmonella.
Thesereac-tionsarebasedonthecleavageofachromogenicsubstratewhichresultsinavisiblecolorchange(seeTable4).
NewdeadlytoolsofSalmonellahavebeendiscovered,presentingopportunitiesfornovelapproachesincontrollingSalmonellaoutbreaks.
Salmonellahasthe"knowhow"andthetoolstoinvadeintothemetabolismofhostcells.
Inanewstudy,researchersdetectedabacterialsortingplatform(bacterialtypeIIIpro-teinsecretionsystem)thatorganisedthenecessarypro-teins.
Akeyroleofthiscytoplasmicsortingplatformistolineupthesecretionofproteinsinaspecificordertobeabletotakecontrolofthehostcell'sfunction.
TheplatformusescustomizedchaperonestoorganisethetypeIIIproteinsecretion.
Itorganisesthebuildingupofaneedlecomplexthroughwhichtheeffectorproteinscanlaterbeinjectedintothehostcells.
Thesenewfindingsmayintroducenewopportunitiesfornovelantimicrobialstrategies[1].
Salmonellacontaminationisthesecondleadingcauseoffood-borneillnessworldwide.
ControllingoutbreaksofSalmonellaisanimportanttaskforfoodregulators,restau-rantsandthefoodindustryingeneral.
TheSalmonellafamilyincludesover2,300serotypesofbacte-ria.
However,twotypes,SalmonellaenteritidisandSalmonellatyphimurium,areresponsibleforapproximatelyhalfofallinfectionsinhumans.
MostoutbreaksofSalmonellamaybetracedbacktodairy,poultryandmeatproducts;however,Salmonellacangrowonnearlyanyfood.
Chicken,eggsandtheirderivativeproductsposeaparticularlyhighrisk.
Kingdom:BacteriaPhylum:ProteobacteriaClass:GammaProteobacteriaOrder:EnterobacterialesFamily:EnterobacteriaceaeGenus:SalmonellaTable1ScientificclassificationMicrobiologicalcontrolinthefoodindustryplaysacriticalroleinpreventingSalmonellaoutbreaks.
TestsandmediausedfortheidentificationofSalmonellatakeadvantageofuniqueaspectsofSalmonella'sphysiologyorbiochemistryrelativetoothergenerawithinthefamilyEnterobacteriaceae.
Forexample,bacteriafromthegenusSalmonellaareprimarilyfacultativeanaerobes,oxidase-negative,catalase-positiveandGram-negativerods.
Moststrainsaremotileandfer-mentglucosewithproductionofbothacidandgas.
Salmonella'sTricksandtheirDetectionJvoSiegrist,ProductManagerMicrobiologyivo.
siegrist@sial.
comFigure1Colorizedscanningelectronmicrograph(SEM)revealingthepresenceofasingleGram-negativeSalmonellatyphimuriumbacteriumthathasbeenisolatedfromapureculture(Magnification20000x;CDC-NationalCenterforZoonotic,Vector-Borne,andEntericDiseases(ZVED);JaniceHaneyCarr)Non-selectivepre-enrichmentSelectiveenrichmentSelectiveisolationConfirmationSampleBPW37°C18hrsRVSBroth41.
5°C24hrsMKTTn37°C24hrsMSRV41.
5°C24hrs(48hrsifnegative)XLDAsecondmediaofchoiceSalmonellaChromogenAgar,BGA,XLT4,Hektoen,SS,etc.
BiochemicalTest(e.
g.
TSI)AnnexDNutrientAgar37°C24hrsSerological08105BufferedPeptoneWater(ISO)17173RappaportVassiliadisBroth,modified43052Muller-KauffmannTetrathionateBroth,Base(ISO)92322RappaportVassiliadismedium(base),modified,semi-solid95586XLDAgar01993SalmonellaChromogenAgarSet76721XLT4Agar(Base)70116NutrientAgarNo292499TripleSugarIronAgar(acc.
toISO)51463UreaBroth66304LysineDecarboxylaseBroth62915LysineIronAgar9sigma-aldrich.
com/microbiologyMicrobiologyCarbohydrateFermentationCat.
No.
ofFlukaCarbohydrateDiscsAcidGasAdonitol--55876Arabinose+/-+/-80372Cellobiose--56481Dextrose++/-63367Dulcitol+/-+/-73044Fructose+/-+/-53901Galactose++/-89608Inositol+/-+/-89614Lactose--28816Maltose++/-77653Mannitol++/-94438Mannose+/-+/-94445Melibiose++93196Raffinose--94226Rhamnose+/-+/-93999Salicin--92971Sorbitol++/-93998Sucrose--94309Trehalose++/-92961Xylose++/-07411Table2TypicalcarbohydratefermentationabilityofSalmonellaFigure2Microbiologyoffoodandanimalfoodstuffs—HorizontalmethodforthedetectionofSalmonellaspp.
;ISO6579:2002/A1:2007(continuedonpage10)Figure3HiCromeMM10sigma-aldrich.
com/microbiologyMicrobiologyCat.
No.
MediumNon-selectivepre-enrichmentbroth08105BufferedPeptoneWater(ISO)D3435Dey-EngleyNeutralizingBroth70123NutrientBrothNo.
278104NutrientBrothNo.
503856NutrientBrothNo.
417181NutrientBrothpH6.
9withoutNaCl77185PeptoneWater94217PeptoneWater,phosphate-buffered(ready-to-usemediainthebottle)77187PeptoneWater,phosphate-buffered67331PeptoneWater,phosphate-bufferedwithFerrioxamineE40893PeptoneWater,phosphate-buffered,Vegitone07507TryptoneWater(ready-to-usemediainthebottle)70194Tryptonewater91366UniversalPre-EnrichmentBrothSelectiveenrichmentbroth69965MosselBroth43052Muller-KauffmannTetrathionateBroth,Base(ISO)04584RappaportVassiliadisBrothacc.
toDINENISO6579:200217173RappaportVassiliadisBroth,modifiedR0773RappaportVassiliadisMedium92322RappaportVassiliadismedium(base),modified,semi-solid84370SalmonellaEnrichmentBroth70153SeleniteBroth(Base)84922SeleniteCystineBroth86352TBGBroth88151TetrathionateBrothSelectiveconfirmationmedia95388BismuthsulfiteAgarB1801BrilliantGreenAgarmodified70134BrilliantGreenAgar,modified16026BrilliantGreenPhenolRedLactoseSucroseAgar70135DCLSAgar90035DCLSAgarNo.
2D7809DeoxycholateCitrateAgar51490HektoenEntericAgar61792LeifsonAgar81648PrilMannitolAgar84368SalmonellaAgaraccordingtonz84369SalmonellaChromogenAgar01993SalmonellaChromogenAgarSet85640SS-Agar95586XLDAgar76721XLT4Agar(Base)Cat.
No.
MediumGrowthandpurificationmedia01477NutrientAgarNo2(readytousemediainthebottle)70116NutrientAgarNo2N9405NutrientAgarpH6.
817209R-2AAgar17221TryptoneYeastextractAgarConfirmationmediaA0715AndradePeptoneWater28943AndradePeptoneWater,Vegitone36408BromcresolPurpleBrothD2935DecarboxylaseBrothBase,Moeller60787KliglerAgar66304LysineDecarboxylaseBroth62915LysineIronAgar39484MethylRedVogesProskauerBroth69150MethylRedVogesProskauerSalineBrothM1053MotilityTestMedium72548NitrateBroth75315OFTestNutrientAgar85438SIMMedium44940TripleSugarIronAgar92499TripleSugarIronAgar(acc.
toISO)51463UreaBrothTable3SalmonellaselectiveanddifferentialmediaBrandCat.
No.
NameFluka00563HiCromeMMAgarFluka90918HiCromeRajHansMedium,ModifiedFluka78419HiCromeSalmonellaAgarFluka05538HiCromeSalmonellaAgar,ImprovedFluka84369SalmonellaChromogenAgarFluka01993SalmonellaChromogenAgarSetTable4ChromogenicmediaforSalmonellaReference:[1]MaríaLara-Tejero,JunyaKato,SamuelWagner,XiaoyunLiu,andJorgeE.
Galán.
ASortingPlatformDeterminestheOrderofProteinSecretioninBacterialTypeIIISystems.
Science,3February2011.
11sigma-aldrich.
com/derivatizationDerivatizationNewDerivatizationReagentsTheprimaryuseofderivatizationisthechemicalmodificationofacompoundbyderivatizingthefunctionalgroup(e.
g.
-OH,-COOH,-NH,and-SH)topromotetheuseofchromatographicanalysis.
Ifleftunderivatized,thesecom-poundscandemonstratepoorchromatographicbehavior,insuf-ficientvolatility,andpoorthermalstabilityorhaveinadequatedetectorresponse.
Bychemicallymodifyingthesecompoundsintoderivatives,theygainpropertiesamenableforchromatographicseparationandaccurateanalysis.
Withourbroadportfolioofderivatizationreagents,weatSigma-Aldrichdemonstrateourcommitmenttowardsseekingnewadvancementsandimple-mentingtheminimprovedandinnovativeproducts.
Checkoutourlatestdevelopmentsthatwillenableyoutoexperienceimprovedperformanceandachievesolutionsforchallengingchromatography.
BrandProductDescriptionPacksizeHPLCDerivatizationenhancedsensitivityinelectrochemicaldetection,analysisofsteroidsFLUKA95159Ferrocenecarboxaldehyde100mgFLUKA56257Ferroceneboronicacid100mgFLUKA89111N-Ferrocenyl-maleimide100mgFLUKA767373-Ferrocenylpropionicanhydride100mgFLUKA50203Ferrocenoylazide100mgHPLCDerivatisationforprimaryaminesanddiaminesFLUKA495582.
6-Dimethyl-4-quinolinecarboxylicacidN-hydroxysuccinimideester100mgHPLC-UVDerivatization:synthesisofwater-solubleprodrugsoflipophilicalcohols,phenolsandaminesFLUKA86546Dibenzylchloromethylphosphate1gDerivatizationofnonsteroidalanti-inflammatorydrugsFLUKA68768N-Methyl-N-(trimethyl-d9-silyl)trifluoroacetamide500μLSilylationforGC-DerivatizationwithoutsolventorexcessofreagentFLUKA79271Trimethylsilylmethallylsulfinate,forGCderivatization5mLFLUKA79264Triethylsilylmethallylsulfinate,forGCderivatization5mLFLUKA79262tert-Butyldimethylsilylmethallylsulfinate,forGCderivatization5mLForfurtherinformation,pleasevisitsigma-aldrich.
com/derivatizationMichaelKiselewsky,ProductManagerAnalyticalReagentsmichael.
kiselewsky@sial.
comMichaelJeitziner,MarketSegmentManagerAnalyticalReagents&Standardsmichael.
jeitziner@sial.
com12sigma-aldrich.
com/lc-msChromatographyobtainedfromafasthighthroughputmethodusingonlyashort2.
1x5mmAscentisExpressC18column.
Althoughthetotalrun-timeisonly1min.
,allmajormatrixcompoundsareseparatedfromtheanalyte,whichisnecessarytooptimizethelimitofdetectionandeliminatesuppressioneffects.
AcomparableseparationonastandardHPLCsystemisnotpossibleorrequiresextensivemodificationstotheHPLCsys-temtominimizepeakdispersionandlossofsensitivity.
Figure2showsthedifferencebetweenastandardHPLCcolumnandaSupelcoAscentisExpresscolumnwithFused-Coreparticles.
UHPLCoroptimizedHPLCsystemswithcore-shellparticlecolumnsareabletoseparatecom-poundsintoverynarrowfractionshavinghighpeakresponsesfromUV,MSorotherdetectors.
Thisadvantagerequiresaveryhighandstablequalityforsolventsandadditives.
Evenaslightimpuritymayresultinadditionalpeakswhichmaycreateacomplicatingissuewithsteepandfastgradientruns(Figure3).
Sincetheearly1940s,liquidchromatographyhaspro-gressedthroughrapiddevelopment.
Evenintheearliestpublications,smallerpackingparticlesandhighercolumnpressureswerebeingproposedforgreaterseparationeffi-cienciesandfasterrun-times.
YearsbeforetheintroductionofacommercialUltraHighPerformanceLiquidChromato-graphy(UHPLC)systembyWatersin2004,V.
Meyerpre-sentedin1997afastchromatographyofbenzodiazepineswithnonporous1.
5μmparticles,anddemonstratedtheadvantagesofincreasedchromatographicresolutionandspeed[1].
Atthepresenttime,allmajorHPLCmanufactur-ersofferUHPLCsystemsforpressuresupto1200barandminimizedmixingintubingconnectionsandfittings.
Anothermajordevelopmentfocusedontheimprovementofstationaryphases.
Thecombinationofsmallsolidmono-disperseparticlescoatedwithaporousfunctionalizedshell(Fused-Core)hasledtooutstandingcolumnefficienciesandhasopenedupnewtechniquesforstandardHPLCandUHPLCusers,e.
g.
veryfastseparationsonshortcolumns.
TheseparationinFigure1representswelltheclarityofresultsUHPLC–State-of-the-ArtinChromatographySigma-AldrichintroducesLC-MSUltraCHROMASOLVRudolfKhling,LC-MSApplicationScientistrudolf.
koehling@sial.
com13sigma-aldrich.
com/lc-msChromatography506.
238+=171.
104Datestrun_manualinj_1ppm.
d:BPC49.
000-1201.
000+AllMStestrun_manualinj_1ppm.
d:EIC171.
103±0.
01+MS2(506.
230)testrun_manualinj_1ppm.
d:EIC506.
235±0.
01+AllMS0.
20.
40.
60.
81.
0Time[min]0.
00.
51.
01.
52.
02.
5x104Intens.
1171.
103203.
095234.
067277.
106301.
072354.
753398.
1512.
0050100150200100200300400427.
247452.
198500600700m/zOSO2N[M+H]+ChemicalFormula:C30H3NO4S161.
082189.
104229.
119270.
128298.
096351.
149409.
164460.
2091.
100200300Intens.
134.
067546.
399583.
222661.
466689.
499+MS,0.
4-0.
5min#(60-75),-PeakBkgrnd+MS2(506.
230),1.
8-1.
8min#(260-274)OH0.
00.
20.
40.
60.
81.
0x107Intens.
0246x106Intens.
0510152025Time[min]0123456Time[min]1345134540minrun-timewithconventionalC18column,4.
6x100mm,3.
5μm,5μLinjectionvolume.
7.
7minrun-timewithSupelcoAscentisExpressC182.
1x50mm,2.
7μm,0.
6μLinjectionvolume(!
)Figure2BPCandUVtracesofanin-processcontrolsample.
TheuseofFused-Coreparticlesleadstomuchshorterrun-timesandlesssampleandsolventconsumptionwhilemaintainingpeakresolution.
Figure1Estradiolcanbederivatizedwithdansylchloride(Fluka39220)anddetectedbyAPCIasdansylderivative[2].
ExcessivereagentcanbeseparatedfromtheanalytewithashortAscentisExpressC18guardcolumncartridge(Supelco53501-5).
UsingUHPLCallowsacompletechromatographyevenwiththisshortcolumn(2.
1x5mm!
).
Theanalysisof10ppbestradiolresultedinaS/N=60(MSandMRM).
(continuedonpage14)1414sigma-aldrich.
com/lc-msChromatographyBrandProductNameDescriptionPacksizeFluka14261AcetonitrileLC-MSUltraCHROMASOLV,≥99.
9%,testedforUHPLC-MS1L,2LFluka14262MethanolLC-MSUltraCHROMASOLV,≥99.
9%,testedforUHPLC-MS1L,2LFluka14263WaterLC-MSUltraCHROMASOLV,testedforUHPLC-MS1L,2LFluka14264TrifluoroaceticacidLC-MSUltraeluentadditive,≥99.
0%suitableforUHPLC-MS1mL,2mLFluka14265FormicacidLC-MSUltraeluentadditive,≥98%suitableforUHPLC-MS1mL,2mLFluka14266AmmoniumformateLC-MSUltraeluentadditive,suitableforUHPLC-MS25gFluka14267AmmoniumacetateLC-MSUltraeluentadditive,suitableforUHPLC-MS25gTable1NewLC-MSUltraCHROMASOLVsolventsandLC-MSUltraeluentadditives.
Reference:[1]Meyer,V.
PraxisderHochleistungs-Flüssigchromatographie,1.
Aufl.
,Wiley-VCH,Weinheim,2004.
[2]Nelson,R.
E.
,etal.
ClinicalChemistry2004,50(2),373–384.
Figure3Standardgradientgradeacetonitrilequality(blue)comparedtoournewLC-MSUltraCHROMASOLVFluka14261(red)underequalconditions(gradientfrom0to100%acetonitrilewithin2min).
Inbothcases,LC-MSUltraCHROMASOLVWater,Fluka14263,isusedasaqueousphase.
Incombinationwithverysensitivedetectionsystems,e.
g.
UVdetectorswithfiberoptics,focusingquadropols,ortime-of-flightoriontrapmassspectrometers,UHPLCsetsnewlimitsforthepurityofsolventsandtheadditivesusedasmobilephasebuffers.
Generally,thisisamuchmorechallengingtaskthantheremovalofparticles.
-2.
50.
02.
55.
07.
510.
0Intens.
[mAU]-5.
00.
00.
51.
01.
52.
02.
53.
03.
54.
04.
55.
0Time[min]15sigma-aldrich.
com/selectophoreNewProductCornerNewSELECTOPHOREIonophoreswithImprovedPropertiesMichaelJeitziner,MarketSegmentManagerAnalyticalReagents&Standardsmichael.
jeitziner@sial.
comTheperformanceofchemicalsensordevicesdependsonthree"S"factors:Selectivity,SensitivityandStability.
Theionophoreplaysthemostcriticalroleinoptimizingthesefactors(seeFigure1).
Sigma-Aldrichhassuccessfullydevelopedandintro-ducedmanynewionophoreswithimprovedcharacteristicsoverpreviouslyexistingones.
TheFlukabrandedionophoresareapplicationtestedusingtheelectrodebodyIS-561,Fluka45137.
Twoexamplesofionophoreswithimprovedpropertiesarelistedbelow.
MagnesiumIonophoreVI,Selectophorefunctiontested,Fluka63112ETH5506,1,3,5-Tris[10-(1-adamantyl)-7,9-dioxo-6,10-diazaundecyl]benzeneThismagnesium-selectiveionophoreishighlylipophilic(logPTLC=8.
5)andobtainssufficientselectivitiesforMg2+againstthemaininterferingcations;therefore,itcanbeusedformagnesiummeasurementeveninserumsamples.
Thisionophorehasalinearresponsebetween110-6Mand610-2Mmagnesiumion.
NitrateionophoreVI,Selectophorefunctiontested,Fluka07295(9-Hexadecyl-1,7,11,17-tetraoxa-2,6,12,16-tetraazacycloeicosane)NitrateionophoreVIisthebestnitrate-selectiveionophoreavailable.
ThePVCmembranestabilityisimprovedbythisionophoreduetothehighlipophilicityofthehexadecylgroup(logP=8.
3(calc.
)).
Themembraneobtainsalinearresponsebetween510-6Mand0.
1Mnitrateion.
SensitivitySelectivityStabilityHNHNHNNNOOOONOOHNOONHOHNONHCH2(CH2)14CH3NNHNHNNNHNHNNHHNOOONONCH3CH3Figure1MagicTriangle:KeyPerformanceParametersofChemicalSensorsFigure2MagnesiumionophoreVIIFigure3NitrateionophoreVIFigure4LeadionophoreVIIIFigure5Iron(III)ionophoreVILeadionophoreVIII,Selectophorefunctiontested,Fluka61796Thisionophoreobtainsexcellentselectivitypropertiesandisthereforeusedwithinthediagnosisofclinicaldisordersaswellasinthemonitoringofenvironmentalsamples.
RecommendedMembraneComposition:10.
0wt%NitrateionophoreVI(07295)46.
0wt%Dibutylphthalate(80100)0.
5wt%Tetraoctylammoniumchloride(87985)43.
5wt%Poly(vinylchloride)highmolecularweight(81392)References:63112MagnesiumionophoreVIO'Donnell,J.
,etal.
,Anal.
Chim.
Acta281,129-134,1993,07295NitrateionophoreVIunpublished.
61796LeadionophoreVIIIW.
-J.
Zangetal.
,AnalyticalLetters40,2007,1023–35.
42942IronionohoreVIR.
Malekietal.
,Turk.
J.
Chem.
33,2009,1–10.
IronionophoreVI,Selectophorefunctiontested,Fluka42942ThenewIron(III)ionophoreVIobtainsanextendedlinearrangeandsuperiorselectivityproperties.
Itcanbethere-foreusedforclinicalanalysisaswellasforenvironmentalanalysis.
Orderafreecopyofourguideon"Selectophore–IonSensorMaterials"atourwebsite:sigma-aldrich.
com/selectophoreorreplyusingtheenclosedBRC.
16Chromatographysigma-aldrich.
com/gc-hsNewHeadspaceGradeSolventsMichaelKiselewsky,ProductManagerAnalyticalReagentsmichael.
kiselewsky@sial.
comWhendevelopingaGC-HSmethod,parameterssuchassamplesolvent,extractiontemperature,extractiontime,samplevolumeandheadspacevolumeareoptimized.
Sigma-AldrichhasdevelopedsolventsspecificallyforGC-HSapplications.
ThepurityandhandlingspecificationsforthesesolventsmeettherequirementsoftheEuropeanPharmacopoeia(Ph.
Eur.
)andUnitedStatesPharmacopeia(USP),aswellasICHguidelines.
ThenewGC-HSproductlineincludeswaterandthreeofthemostcommonlyusedorganicsolvents:dimethylsulfoxide(DMSO),N,N-dimethyl-formamide,andN,N-dimethylacetamide.
N,N-dimethylfor-mamideanddimethylsulfoxidearespecifiedinPh.
Eur.
andUSPforwater-insolublesubstances.
Wateristhepreferredsolventforwater-solublesolutions,asdescribedinPh.
Eur.
andUSPmonographs.
Inaddition,Sigma-AldrichhasnowexpandeditsGC-HSportfoliowithtwonewproducts,GC-HSCyclohexaneand1-Methyl-2-pyrrolidinone.
Allsolventsaremicrofilteredat0.
2μmandpackedunderinertgasforextendedshelflife.
Literature[1]UnitedStatesPharmacopeia,31stEdition(2008),ResidualSolvents.
[2]Ph.
Eur.
6.
0(2008)Method2.
4.
24,Identificationandcontrolofresidualsolvents.
[3]ICHGuidelineQ3C,Impurities:GuidelineforResidualSolvents,TheFourthInternationalConferenceonHarmonization,July17,1997.
Cat.
No.
BrandProductNameAbbreviationBPPacksizeNEW68809FlukaCyclohexanone,forGC-HS-155°C1L44901FlukaN,N-Dimethylacetamide,forGC-HSDMA166°C1L51781FlukaN,N-Dimethylformamide,forGC-HSDMF153°C1L67484Fluka1,3-Dimethyl-2-imidazolidinone,forGC-HSDMI225°C100mL,1L51770FlukaDimethylsulfoxide,forGC-HSDMSO189°C1LNEW69337Fluka1-Methyl-2-pyrrolidinone,forGC-HSNMP202°C1L53463FlukaWater,forGC-HS-100°C1LProducttableSolventsforGCHeadspaceAnalysisFormoreinformation,pleasevisitourwebsite:sigma-aldrich.
com/gc-hsSubscribetodaytoreceivetheFlukaeNewsletterStayabreastofthelatestinnovations,applications,promotionsandregionalactivitiesinanalytical/chromatographydisciplinesfromSigma-Aldrichbysigningupforourelectronicnewsletter.
OurmonthlyFlukaeNewsletterbringsyouabriefcompilationofproductinformation,applicationtips,andpromotionaloffersrelatedtoreagentsandstandardsforTitrationSpectroscopyChromatographyMicrobiologyLabwareMonthlySavingsSignupatsigma-aldrich.
com/analytical_newsletter17sigma-aldrich.
com/standardsStandardsDAIH-andDNPH-AldehydeandKetoneStandardsIngridHayenga,SeniorChemist,R&DEuropeingrid.
hayenga@sial.
comThefollowingtableprovidesasummaryofthemostimportantderivatizingagentsaswellastheiradvantagesanddisadvantages[2].
ReagentsAnalyticalmethodAdvantageDisadvantageAirsamplingtechniquesa2.
4-Dinitrophenylhydrazine(DNPH)HPLC-UV,HPLC-MS,(GC-FID,CE)Internationalstandardprocedure;largevarietyofapplicationsavailable;reagentsandderivativesstableInterferenceswithairborneoxidants(Nox,O3);limitedsensitivityI,Cb,D,PSDHantzschreagentUV,fluorescence,HPLC-UV,HPLC-fluorescenceWellsuitableforon-lineanalysis;fluorescencedetectionSlowandnon-quantitativereaction;limitedtoaliphaticcarbonylsI,flow-throughanalyzersChromotropicacid+pararosanilineUV/VisOnlyreadilyavailableinstrumentationrequiredSuitableonlyforformaldehydeI4-nitrophenyl-hydrazine(pNPH)HPLC-UVSlightlyred-shiftedabsorptionmaximaofthederivativescomparedtotheDNP-hydrazonesReplacedbyDNPHbecauseofitsfasterderivatizationreactionC,IHalogenatedaromatichydrazinesandhydroxylaminesGC-ECD,GC-FID,GC-MSImprovedchromatographicresolutioncomparedtoHPLCSlowreactionswithcarbonyls;EandZisomersseparatedC,IN-methyl-benzothiazolon-(2)-hydrazone(MBTH)4-Amino-3-hydrazino-5-mercapto-1,2,4-triazol(Purpald)UV/Vis,HPLC-UVOnlyreadilyavailableinstrumentationrequiredSelectiveforformaldehydebutcross-selectivitytootheraldehydesIDansylhydrazine(DNSH)HPLC-fluorescenceLowlimitsofdetectionInstabilityofDNSHanditsderivativestowardshydrolysisC,IN-Methyl-4-hydrazino-7-nitrobenzofuran(MNBDH)HPLC-UV,HPLC-MSSlightlyfasterreactionwithcarbonylcompounds,higherselectivityandlowerdetectionlimitscomparedtoDNPHaswellasotherN-alkylatedhydrazinereagentsC,I,PSDa:C=cartridge,I=impinger,D=denuder,PSD=passivesamplingdevicesb:reagentcoatedcartridgesarecommerciallyavailableThemostrelevantDNPH-andDAIH-aldehydeandketonestandardsareavailableatSigma-Aldricheitherassolutionsoraspuresubstances,asanalyticalstandardsorasBCRcertifiedreferencematerials.
Formaldehydeandacetaldehydearekeycomponentsofphotochemicallygeneratedairpollution.
Oxidationofvola-tileorganiccompounds(VOC)byreactionofOHradicalsisconsideredtobetheirpredominantsource,buttheyarealsoemitteddirectlyintotheurbanatmosphereduringtheincompletecombustionoffossilfuels.
Ithasbeenassumedthatthesetwoimportantintermediatespeciesaccountforupto90%ofthetotalaldehydesinair[1].
Forshortchainaldehydesandketones,anumberofderivatizationreagentshavebeendeveloped.
Theirdetectionisperformedbyphotometryorfluorescence,e.
g.
reactionwithchromotropicacidorpararosaniline.
Thesereactionsarevalidifasumparameteristobeobtained;however,theirmajordrawbackistheinabilitytodeterminedifferentcarbonylssimultaneouslywithinonesample.
TheoxidativecouplingofaldehydeswithtwomoleculesofN-methyl-benzothiazolon-(2)-hydrazone(MBTH)leadstoanintensivelycoloredproduct.
Althoughitispossibletodeterminedifferentaldehydesandketoneswiththismethod,itsselectivitydependsheavilyontheanalytestructureandtheexperimentalconditions.
Therefore,toachievespeciationinformation,achromato-graphicseparationisrequired.
Foratmosphericdetectionofshortchainaldehydesandketones,theuseofimpreg-natedsilica-gelcartridgeshasprovidedgoodsensitivity,theimpregnatingreagentsbeing2-diphenylacethyl-12.
3-indandione-1-hydrazone(DAIH)or2.
4-dinitrophenyl-hydrazone(DNPH).
Thesereagentsarealsoapplicableasprecolumnderivatizingreagentsforliquidphaseanalysis.
[2](continuedonpage18)18Standardssigma-aldrich.
com/standardsCat.
No.
ProductDescriptionPackSize473442-Butanone-2.
4-DNPHsolution100μg/mlinacetonitrileampuleof1ml47340-UAcetaldehyde-2.
4-DNPHsolution1000μg/mlinacetonitrileampuleof1ml4M7340-UAcetaldehyde-2.
4-DNPHsolution1000μg/mlinacetonitrilepkgof5ampules(1mleach)47341Acetone-2.
4-DNPHsolution1000μg/mlinacetonitrileampuleof1ml4M7341Acetone-2.
4-DNPHsolutions1000μg/mlinacetonitrilepkgof5ampules(1mleach)47342Acrolein-2.
4-DNPHsolution1000μg/mlinacetonitrileampuleof1ml4M7258-UAldehyde/ketone-DNPHTO11/IP-6AMix15μg/mleachcomponentinacetonitrilepkgof3ampules(1mleach)47343Benzaldehyde-2.
4-DNPHsolutions100μg/mlampuleof1ml47345-UButyraldehyde-2.
4-DNPHsolution1000μg/mlampuleof1ml47649-UCARBcarbonyl-DNPHMix1Inacetonitrile(varied)ampuleof1ml47650-UCARBMethod1004DNPHMix13μg/mlinacetonitrileampuleof1ml47651-UCARBMethod1004DNPHMix22μg/mlinacetonitrileampuleof1ml47672-UCarbonylDNPHMix120μg/mlinacetonitrileampuleof1ml47671-UCarbonylDNPHMix22μg/mlinacetonitrileampuleof1ml47175-UCrotonaldehyde-2.
4-DNPHsolution100μg/mlinacetonitrileampuleof1ml47674-UCyclohexanone-2.
4-DNPHsolution500μg/mlinacetonitrileampuleof1ml48149-UEPATO-11ASixComponentCarbonyl-DNPHMix15μg/mleachcomponentinacetonitrilepkgof1.
5ml47177Formaldehyde-2.
4-DNPHsolution100μg/mlinacetonitrileampuleof1ml47564-UGlutaraldehyde-2.
4-DNPHsolution100μg/mlinacetonitrileampuleof1mlOR2R1O2NNO2HNNH2O2NNO2HNNR2R1OR2R1NH2NOONNOOR1R2Figure1Derivatizationofcarbonylcompoundswith2.
4-dinitrophenylhydrazone(DNPH)Figure2Derivatizationofcarbonylcompoundswith2-Diphenylacetyl-1.
3-indandione-1-hydrazoneCat.
No.
ProductPacksize14423AcetaldehydeDAIHderivative50mg02819Acetone,DAIHderivative50mg13173Acroleine,DAIHderivative50mg55556Crotonaldehyde,DAIHderivative50mg91547Cyclohexanone,DAIHderivative50mg06947Formaldehyde,DAIHderivative50mg51299Propionaldehyde,DAIHderivative50mg442321-U2.
5-Dimethylbenzaldehyde-2.
4-DNPHampuleof100mg4423392-Butanone-2.
4-DNPHampuleof100mg442434Acetaldehyde-2.
4-DNPHampuleof100mg442436Acetone-2.
4-DNPHampuleof50mg442441Acrolein-2.
4-DNPHampuleof25mg442469Benzaldehyde-2.
4-DNPHampuleof100mg442504Butyraldehyde-2.
4-DNPHampuleof100mg442529Crotonaldehyde-2.
4-DNPHampuleof100mg442533Cyclohexanone-2.
4-DNPHampuleof100mgTable1DAIH-andDNPH–standards,puresubstanceCat.
No.
ProductDescriptionPacksize33852Decanal2.
4-DNPH>98.
5%10mg,100mg442597Formaldehyde-2.
4-DNPHampuleof100mg33848Heptanal2.
4-DNPH>98.
5%100mg442614Hexaldehyde-2.
4-DNPHampuleof100mg442639Methacrolein-2.
4-DNPHampuleof100mg33851Nonanal2.
4-DNPH>98.
5%100mg33849Octanal2.
4-DNPH>98.
5%100mg442722o-Tolualdehyde-2.
4-DNPHampuleof100mg442768Propionaldehyde-2.
4-DNPHampuleof100mg442735p-Tolualdehyde-2.
4-DNPHampuleof100mg34396Succinaldehyde>98.
5%50mg442834Valeraldehyde-2.
4-DNPHampuleof100mg(continuedonpage19)19sigma-aldrich.
com/standardsStandardsNewAnalyticalStandardsfortheAnalysisofHerbalMedicinalProductsMatthiasNold,ProductManagerAnalyticalStandardsmatthias.
nold@sial.
comHerbalmedicinalproducts,pharmaceuticalproductswhicharederivedfrommedicinalplants,areverypopularasanalternativetosyntheticdrugs.
Inrecentyears,regulatorypressureforherbalmedicinalproductshasincreased,resultingintheneedformonitoringtheconcentrationsofactiveingredientsandothercharacteristiccomponents.
Sigma-Aldrichoffersanalyticalstandardsaswellasprimaryreferencestandardsofactiveingredientsandmarkercom-poundsofmedicinalplants.
Thisportfolioofproductscon-tinuestoexpandataquickpace.
JustaswepresentedseveralnewproductsinthefirsttwoissuesofAnalytixin2011,weareonceagainintroducingnewadditionstothisrapidlygrowingproductline.
Ourwebpageatsigma-aldrich.
com/medicinalplantscontainsanup-to-datelistingoftheseproductscataloguednotonlybyalphabeticalorder,butalsoaccordingtosub-stanceclassandbygenusforawidearrayofmedicinalplants.
Cat.
No.
BrandDescriptionPackSize42251FlukaApigenin10mg91466FlukaBetulinicacid10mg43412Fluka(+)Catechin10mg95082FlukaChrysin50mg06536Flukatrans-Cinnamaldehyde50mg97013Flukatrans-Cinnamicacid50mg38907FlukaIsorhamnetin10mg69545FlukaKaempferide10mg96353FlukaKaempferol10mg49968FlukaLuteolin-7-glucoside10mg06279FlukaMangiferin10mg28660FlukaProcyanidinA210mg16654FlukaQuercetin3-glucoside10mg69686FlukaShikimicacid50mgTable1Newanalyticalstandardsandcertifiedreferencematerials(CRMs)ofactiveingredientsandmarkersubstancesfortheanalysisofherbalmedicinaldrugsCat.
No.
ProductDescriptionPackSize47178-UHexaldehyde-2.
4-DNPHsolution1000μg/mlinacetonitrileampuleof1ml47886Isobutyraldehyde-2.
4-DNPHsolution100μg/mlinacetonitrileampuleof1ml47179Isovaleraldehyde-2.
4-DNPHsolution1000μg/mlinacetonitrileampuleof1ml47180-UMethacrolein-2.
4-DNPHsolutions100μg/mlinacetonitrileampuleof1ml47183m-Toluoaldehyde-2.
4-DNPHsolution100μg/mlinacetonitrileampuleof1ml47032-Uo-Phthaldialdehyde-(DNPH)2solution10μg/mlinacetonitrile:DMSO(7:3)pkgof3x2ml47182o-Tolualdehyde-2.
4-DNPHsolution100μg/mlampuleof1ml47181Propionaldehyde-2.
4-DNPHsolution1000μg/mlampuleof1ml47184-Up-Tolualdehyde-2.
4-DNPHsolution100μg/mlampuleof1ml40117-UPyridine-2-Aldehyde-DNPHStandardinacetonitrilepkgof3x2ml40081-UPyridine-4-Aldehyde-DNPHsolution1mMinacetonitrile:DMSO,4:1pkgof3x2ml47285-UTO11/IP-6AAldehyde/Ketone-DNPHMix15μg/mleachcomponentinacetonitrileampuleof1ml47185-UValeraldehyde-2.
4-DNPHsolutions100μg/mlampuleof1mlTable2DAIH-andDNPH-standards,insolutionandmixesCat.
No.
ProductDescriptionPackSizeBCR55122.
4-Dinitrophenylhydrazones,solutionsSetof4xBCR-551and1xBCR-552(blank)setBCR548Acrolein-2.
4-DNPH10mgBCR5534Formaldehyde-2.
4-DNPHonfilterSetof2xBCR-553and1xBCR-554(blank)setBCR550Glutaraldehyde2.
4-DNPH10mgTable3BCRcertifiedreferencematerialReferences:[1]Possanzini,M.
,DiPalo,V.
Chromatographia1997,46,5/6,235.
[2]Vogel,M.
,Büldt,A.
,Karst,U.
,Fresenius,J.
Analy.
Chem.
2000,366,781.
20sigma-aldrich.
com/cspStandardsInorganicCustomStandardsAnInteractiveOnlinePlatformTraceCERTstandardsforAAS,ICPandICareCertifiedReferenceMaterialsfulfillingthehighest-qualitystandards.
*Inadditiontoourcomprehensiveportfolioofcatalogueproductswealsoofferyouacustomservicewhereyoucandefineyourownmulti-componentstandardsatthesamehighquality,usingourInorganicCustomStandardsOnlinePlatform:sigma-aldrich.
com/cspForallTraceCERTCustomStandardsweguarantee:CertificationunderdoubleaccreditationfollowingISO/IEC17025andISOGuide34HighestlevelofaccuracyandreliabilityMinimizeduncertaintiesandlot-specificvaluesTraceabilitytoatleasttwoindependentreferences(i.
e.
NIST,BAMorSIunitkg)PrintedcertificateaccordingtoISOGuide31Light-andgas-tightaluminiumfoilbagpackagingallowinguptofouryears'shelflifeWithafewsimplemouseclicksyoucanspecifythedesiredcharacteristicsamongthefollowing:ElementstandardIonstandardDefiningmatrixAnalytesConcentrationsTheCustomStandardsPlatformisadynamicwebpage:elements,ionsandmatricescanonlybechosenifthecombinationsarechemicallyallowed.
Afteryourrequesthasbeensubmittedonline,wewillevaluatetheproductioncostsandrespondwithaquota-tionbye-mail.
It'seasy,tryitout!
*Atsigma-aldrich.
com/tracecertyoucanfindtheextensiveTraceCERTportfolioofcertifiedsingle-andmulti-elementstandards.
21sigma-aldrich.
com/organiccrmNewProductCornerTheprimaryadvantageof1HquantitativeNMRasarelativeprimarymethodisthattheintegralsoftheprotonsignalsarecompletelyindependentofthechemicalstructure.
Therefore,traceabilitycanbeestablishedbetweentwodif-ferentcompounds,incontrasttomostotheranalyticaltechniques.
WithasmallsetofNISTtraceableinternalstandards,weareabletocertifybasicallyanyorganiccompoundbymeasur-ingagravimetricallyproducedmixtureoftheanalyteandtheinternalstandard.
Theaccuratelydeterminedmasstomassratiothenallowsforthecalculationoftheanalytecontentwithaveryhighlevelofconfidence.
Typicaluncer-taintiesrangefrom0.
5%downto0.
1%.
NeworganicTraceCERTproductsTheportfoliooforganicTraceCERTCRMsintendedforuseaschromatographystandardsiscomprisedofover50prod-uctsandiscontinuallygrowing.
Theproductsincludeaminoacids,PAHs,fattyacids/FAME,pesticidesandphar-maceuticals,aspublishedinpreviousarticles[1].
Themostrecentproductadditionscompriseseveralnatu-ralproductsaslistedbelow.
Pleasevisitourwebsite(sigma-aldrich.
com/organiccrm)whereyoucanfindacompleteandcurrentlistingofallproductsandalibraryoftechnicalarticlesandexamplesofcertificatesthatcanbedownloaded.
Cat.
No.
BrandDescriptionPacksize93485FlukaAMOZ50mg94664FlukaAnhydrotetracyclinHCl50mg51868Flukatrans-Caffeicacid50mg56396FlukaCaffeine100mg52229Flukatrans-Ferulicacid50mg76635FlukaFumaricacid100mg91215FlukaGallicacid100mg52341FlukaSalicylicacid100mg68654FlukaVanillicacid50mgTable1NEWorganicneatCRMsTraceCERTReferences:[1]TraceCERTOrganicCertifiedReferenceMaterials,Analytix,Vol2and3,2010;Vol1,2011.
Foranalyticaltestinglabs,ISO/IEC17025accreditationisgainingincreasedimportancefordemonstratingcompe-tenceintestingandcalibration.
Essentialtothisaccredita-tionistheuseofsuitablecalibrationstandards,withtherecommendationthatthesestandardsaretraceabletointernationallyrecognizedreferencematerials.
Whiletheavailabilityofinorganiccertifiedreferencematerials(CRMs)isusuallyhigh(seeourcorrespondingTraceCERTportfolioatsigma-aldrich.
com/inorganiccrm),therehasbeenalackofsourcesfortraceableorganicCRMs.
Inthelastyear,Sigma-Aldrichhasintroducedtheinnova-tivenewproductlineoforganicTraceCERTstandards[1].
ThesepremiumCRMsarecertifiedinadoubleaccreditedlaboratory,fulfillingbothISO/IEC17025andISOGuide34,usinghigh-performancequantitativeNMR(HP-qNMR)forcontentdeterminationwithdirecttraceabilitytoNISTandSI.
TheorganicTraceCERTreferencematerialsarecharacter-izedby:CertifiedContentbyHP-qNMRSuperiorlevelofaccuracy,calculateduncertaintiesandlot-specificvaluesTraceabilitytoNISTComprehensivedocumentationdeliveredwiththeproduct(certificationaccordingtoISOGuide31)NewTraceCERTOrganicCertifiedReferenceMaterialsMatthiasNold,ProductManagerAnalyticalStandardsmatthias.
nold@sial.
comAlexanderRück,SeniorScientistR&DEuropealexander.
rueck@sial.
comChristineHellriegel,SeniorScientistR&DEuropechristine.
hellriegel@sial.
com22sigma-aldrich.
com/volpacTitrationOur5Land10LVOLPACsolutioncontainersareperfectwhenlargervolumesofready-to-usetitrationsolutionsareneeded.
VOLPACcontainersconsistofaflexiblepolyethylenebagwithanoutlettapandacubiccardboardsupportingframe.
BecauseofVOLPAC'scleverdesign,aircannotenterthecontainerduringthedispensingoperation.
Asaresult,VOLPACcontainerscanbedrainedcompletelywithoutcontaminationforlesswasteandmorereliableanalyses.
AdvantagesofVOLPACcontainers:HighqualityofcontentandpackingEasyhandlingNocontaminationduringdispensingReducedstoragefootprintandpackagingmaterialNew!
AllVOLPACcontainersarenowsuppliedwithtwodifferent-sizedadaptersthatallowdirectconnectionofthetitratingtubetotheVOLPACcontainer.
Cat.
No.
DescriptionAcidsolutions35335-5L-VOLPAC,35335-10L-VPHydrochloricacidsolutionReag.
Ph.
Eur.
0.
1mol/L35329-5L-VP35329-10L-VPHydrochloricacidsolutionReag.
Ph.
Eur.
0.
5mol/L35328-5L-VOLPAC35328-10L-VPHydrochloricacidsolutionReag.
Ph.
Eur.
1mol/L35327-10L-VOLPACHydrochloricacidsolution2mol/L35358-5L-VP35358-10L-VPSulfuricacidsolutionReag.
Ph.
Eur.
0.
05mol/L35357-5L-VP35357-10L-VPSulfuricacidsolutionReag.
Ph.
Eur.
0.
1mol/L35355-10L-VPSulfuricacidsolutionReag.
Ph.
Eur.
0.
25mol/L35354-5L-VOLPAC35354-10L-VPSulfuricacidsolutionReag.
Ph.
Eur.
0.
5mol/L35348-5L-VP35348-10L-VPSulfuricacidsolution2.
5mol/LVolumetricTitrationVOLPACSolutionContainerswithnewadapterAndreaFelgner,ProductManagerAnalyticalReagentsandrea.
felgner@sial.
com23sigma-aldrich.
com/volpacTitrationCat.
No.
DescriptionBasesolutions35116-5L-VPPotassiumhydroxidesolution0.
5mol/L35125-10L-VOLPACPotassiumhydroxidesolution0.
1mol/L35262-10L-VOLPACSodiumhydroxidesolution0.
01mol/L35263-5L-VOLPAC35263-10L-VPSodiumhydroxidesolutionReag.
Ph.
Eur.
0.
1mol/L35256-5L-VOLPAC35256-10L-VPSodiumhydroxidesolutionReag.
Ph.
Eur.
1mol/L35261-10L-VPSodiumhydroxidesolution0.
2mol/L31086-5L-VP31086-10L-VPSodiumhydroxidesolution0.
25mol/L35257-5L-VOLPAC35257-10L-VPSodiumhydroxidesolution0.
5mol/LpHBuffersolutions33665-5L-VP33665-10L-VPBuffersolutionpH4.
0(20°C)withfungicide(citricacid/sodiumhydroxide/sodiumchloride)redcoloredpH4.
033643-5L-VP33643-10L-VPBuffersolutionpH4.
0(20°C)withfungicide(citricacid/sodiumhydroxide/sodiumchloride)pH4.
033666-5L-VP33666-10L-VPBuffersolutionpH7.
0(20°C)withfungicide(potassiumdihydrogenphosphate/disodiumhydrogenphosphate)greencoloredpH7.
033646-5L-VP33646-10L-VPBuffersolutionpH7.
0(20°C)withfungicide(potassiumdihydrogenphosphate/disodiumhydrogenphosphate)pH7.
033667-5L-VP33667-10L-VPBuffersolutionpH9.
0(20°C)(borax/hydrochloricacid)bluecoloredpH9.
033648-5L-VP33648-10L-VPBuffersolutionpH9.
0(20°C)(borax/hydrochloricacid)pH9.
033668-10L-VPBuffersolutionpH10.
0(20°C)(borax/sodiumhydroxide)violetcoloredpH10.
0Complexometricsolutions34544-5L-VPEthylenediaminetetraaceticaciddisodiumsaltsolutionwithzinccomplexadded(solutionB)1mLsolution=1Germandegreeofhardnessin100mLofwater35102-5L-VP35102-10L-VPIDRANALIIIsolution(EDTA-Na2)0.
2mol/L34550-5L-VP-R34550-10L-VP-RIDRANALIIIsolution(EDTA-Na2),Reag.
Ph.
Eur.
0.
1mol/L35103-5L-VP35103-10L-VPIDRANALIVsolution(DCTA-Na4),Reag.
Ph.
Eur.
0.
1mol/LSaltsolutions34631-5L-VPPotassiumdichromatesolutionforCODdeterminationaccordingtoDIN384090.
02mol/L34277-5L-VP-RSodiumcarbonatesolution0.
5mol/L34247-10L-VP-RSodiumfluoridesolution40g/L34246-10L-VP-RSodiumoxalatesolution25g/L35224-5L-VPSodiumthiosulfatesolution,fordeterminationofiodineadsorptionnumberaccordingtoASTMD151034449-10L-VP-RSodiumthiosulfatesolution0.
05mol/L35233-5L-VPSodiumthiosulfatesolution0.
2mol/L35245-5L-VP35245-10L-VPSodiumthiosulfatesolutionReag.
Ph.
Eur.
0.
1mol/L34400-5L-VPLuff-Schoorl-Reagent(CuSO4*5H2O)~25g/LTable1CompletelistofallFlukabrandproductsthatareavailableinVOLPACcontainers(Theseproductscanbeeasilyrecognizedsincetheyaretaggedwitha'-VOLPAC'or'-VP'intheirproductnumber.
)SpecialofferonallVOLPACsolutioncontainers!
Receive45%offyourfirstorderofanyVOLPACcontainer.
Pleasequotepromotioncode979whenplacingyourorder.
OffervaliduntilJuly31,2011.
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