Mass Spec Results In Seconds With Direct Sample …€¢ Insecticide on Mosquito Nets ... •...

MASS SPEC RESULTSIN SECONDS WITHDIRECT SAMPLE ANALYSIS

AxION DSA System A Reference Notebook of DSA Applications—Second Edition, 2013

2www.perkinelmer.com/DSA

REVOLUTIONIZE YOUR MASS SPECWORKFLOW Going from sample to results can often be complex

and time-consuming. That is why PerkinElmer has introduced a unique solution: the AxION® DSA (Direct

Sample Analysis) system. Nothing simplifies workflows more than AxION DSA. Diminish cumbersome method development, eliminate chromatography and dramatically reduce sample preparation.

RESULTS IN SECONDSThe innovative AxION DSA technology was developed for the rapid direct analysis of solid, liquid or gaseous samples. It offers a novel alternative to standard chromatographically interfaced solutions. Laboratories can now screen, compare and confirm virtually any sample, by introducing it directly to a mass spectrometer in a matter of seconds.

• No chromatography required.

• Avoid time consuming method development.

• Minimal sample preparation.

This reference notebook of direct sample analyses, highlights the performance characteristics of the AxION DSA. It features a diverse selection of applications, sample types and results across a broad array of industries.

The AxION DSA system will change the way you work by providing results-driven decisions in seconds.


Index of Applications

• Atrazine in Water ................................................................................................................................................................22

• Carbamates in River Water ..................................................................................................................................................23

• Insecticide on Mosquito Nets ..............................................................................................................................................24

• Personal Care Products in River Water .................................................................................................................................25

ENVIRONMENTAL

• Bisphenol A in plastic ..........................................................................................................................................................26

• Ferulic Acid in Skin Oil .........................................................................................................................................................27

• Fullerene C-60 .....................................................................................................................................................................28

• Limonene in Orange Peel ....................................................................................................................................................29

• Methylparaben in Hair Gel ..................................................................................................................................................30

• Paraben Screening in Texture Cream ...................................................................................................................................31

• Parabens in Lipstick .............................................................................................................................................................32

• Parabens in Lotions .............................................................................................................................................................33

• Salicylic Acid in Foundation .................................................................................................................................................34

CHEMICAL

FOOD AND BEVERAGE• Caffeine in Decaffeinated Coffee ..........................................................................................................................................5

• Caffeine in Green Teas ..........................................................................................................................................................6

• Capsaicin and Dihydrocapsaicin in Peppers ...........................................................................................................................7

• Curcumins in Turmeric Powder ..............................................................................................................................................8

• DEHP in Mango Juice ............................................................................................................................................................9

• Fungicide on Apple Peel ......................................................................................................................................................10

• Fungicide on Lemon Peel .................................................................................................................................................... 11

• Fungicides on Oranges ........................................................................................................................................................ 12

• Malathion on Peaches ......................................................................................................................................................... 13

• Melatonin in Lazy Cake® .....................................................................................................................................................14

• Natural Vanilla Extract ......................................................................................................................................................... 15

• Olive Oil Adulteration ..........................................................................................................................................................16

• Pomegranate Juice Adulteration ......................................................................................................................................... 17

• Propanethiol S-oxide in Onions ...........................................................................................................................................18

• Resveratrol in Red Wine ......................................................................................................................................................19

• Sterols in Olive Oil ...............................................................................................................................................................20

• Sweeteners in Diet Cola ......................................................................................................................................................21


Index of Applications

• Components of Multivitamin Powder .................................................................................................................................. 41

• Aerosols/Inalers ...................................................................................................................................................... 42

• Components of Panadol® Extra ............................................................................................................................... 43

• Components of Panadol® Sinus Max ........................................................................................................................44

• Paracetamol Tablets ................................................................................................................................................ 45

NUTRACEUTICAL

PHARMACEUTICAL

FORENSICS• Cathinones in Bath Salts .....................................................................................................................................................35

• CID of Cathinone Standards ................................................................................................................................................36

• Date Rape Drug in Cola .......................................................................................................................................................37

• Ethyl Centralite ....................................................................................................................................................................38

• Nitroglycerin .......................................................................................................................................................................39

• Testosterone in Steroid Powder ...........................................................................................................................................40


TOF MS

DIRECT SAMPLE ANALYSIS

Easy to use

Product integrity

No chromatography

• Caffeineisanaturalstimulantinteaandcoffee

• Decaffeinatedcoffeeofferspeoplethechoicetoavoidcaffeineorreducetheircaffeineintake

• DSA/TOFanalysisofdecaffeinatedcoffeeconfirmedcaffeinewasstillpresentwithhighaccuratemass

• Analysiswasperformedin15seconds;confirmedproductcontaminationwithnosamplepreparationandexternalcalibration

Food and Beverage: Caffeine in Decaffeinated Coffee


TOF MS


Rapid analysis

Comparison of products

No method development

Food and Beverage: Caffeine in Green Teas

• Caffeineisanaturalstimulantenjoyedbymanyinteaandcoffee

• RapidscreeningofdifferentgreenteasbyDSA/TOFenableseasyproductcomparisons

• Analysiswasperformedin15secondswithnosamplepreparationandexternalcalibration


TOF MS


No sample preparation

Easy to use

Semi-quantitative

• Capsaicinanddihydrocapsaicinarethecompoundsresponsibleforpepperhotness

• 1cm3piecesofcubanelle,chilli,andjalapeñopeppersweredirectlyanalyzed

• Thesignalintensitiesprovidedtherelativeamountsofcapsaicinanddihydrocapsaicininthepeppers


Food and Beverage: Capsaicin and Dihydrocapsaicin in Peppers


TOF MS



Easy to use

Complete characterization

• Curcuminsaretheactiveingredientinturmericpowderusedforfoodflavoring,dyeing,andpossiblemedicalbenefits

• Turmericpowderwasdirectlyanalyzedinaglasscapillary

• DSA/TOFanalysisofturmericpowderdetectsall3curcuminoidswithhighmassaccuracy


Food and Beverage: Curcumins in Turmeric Powder


TOF MS


Food and Beverage: DEHP in Mango Juice

Results in seconds


Assures food safety

• Bis-(2-Ethylhexyl)Phthalate(DEHP),bannedbytheEU,hasbeenusedasacheaperalternativecloudingagenttoimprovetheappearanceoffruitjuice

• DEHPhasbeenaddedillegallytoexoticfruitjuices,suchasmangoandpassionfruit.Themaximumallowablelimitforphthalatesinfruitjuiceis1ppm

• PresenceofDEHPat1ppmwasconfirmedin15secondswithnosamplepreparation,chromatographyorexternalcalibration


TOF MS


Easy to use

Fast accurate mass

Assures food safety

• Thiabendazoleisacommoningredientinthewaxesappliedtotheskinsofcitrusfruitsandisalsoafungicideusedtoprotectharvestyields

• ResidualthiabendazolewasconfirmedusingDSA/TOFwithhighmassaccuracy

• Analysisperformedin15secondswithnosamplepreparationandexternalcalibration

Food and Beverage: Fungicide on Apple Peel


TOF MS


Outstanding sensitivity

Fast accurate mass

Assures food safety

• Pesticidessuchasimazalilareoftenusedtoprotectfruitsandvegetablesfrominsects

• Awashed1cm3pieceoflemonpeelwasextractedwithmethanolandanalyzed

• Residualimazalilwasconfirmedwithhighmassaccuracy

• Analysiswasperformedin15secondswithminimalsamplepreparationandexternalcalibration

Food and Beverage: Fungicide on Lemon Peel


TOF MS



Easy to use

Assures food safety

• Tracesoffungicidesonourfoodposeapotentialrisktohumanhealth

• Swabbingwithmethanolfromanorangeboughtatagrocerystorewasanalyzed

• DSA/TOFanalysisdetectedthepresenceoftwofungicidesontheorangeskin


Food and Beverage: Fungicides on Oranges


TOF MS


Easy to use

Low detection limits

Fast, accurate mass

• Malathionisacommonlyusedinsecticide.TheEPAtolerancelevelformalathiononpeachesis8000ng/g

• Apeachsurfacewasspikedwith10ng/gmalathion,thenswabbedwithmethanolandanalyzed

• DSA/TOFanalysisoftheswabsampleconfirmedmalathion,withhighmassaccuracy,at800timeslowerthantheEPAtolerancelevel


Food and Beverage: Malathion on Peaches


TOF MS



Confirms active ingredient

Rapid analysis

• LazyCakes®,marketedas“relaxationbrownies”arelacedwiththesleepaidmelatonin

• Packagingiskid-friendlyandchildrenhaveeatenthemandfallenasleep

• Apieceofcakewasanalyzedtodeterminetheingredientthatwascausingsleepiness

• Directanalysisconfirmstheactiveingredientmelatoninwithhighmassaccuracy


Food and Beverage: Melatonin in Lazy Cake®


DIRECT SAMPLE ANALYSISTOF MS


Results in seconds

Easy to use

Assures product authenticity

Food and Beverage: Natural Vanilla Extract

• Thepriceofnaturalvanillaextractisupto5timesmoreexpensivethanartificialvanillaflavoring

• 4-hydroxbenzaldehydecanbeusedasamarkerionasitispresentinnaturalvanillaextractbutnotinartificialvanillaflavorings

• DSA/TOFanalysis,performedin15seconds,rapidlyconfirmsproductauthenticitywithnosamplepreparationandexternalcalibration


TOF MS


Results in seconds

No chromatography


Food and Beverage: Olive Oil Adulteration

• Oliveoilisonethemostadulteratedfoodproductsinworld.Itis4-5timesmoreexpensivethansoybasedvegetableoil

• Ratiooflinoleicacidtooleicacidresponsecanbeusedasawaytodetectadulterationofoliveoil


Adulterated Olive Oil with Soy Based Oil.

Olive Oil


TOF MS


Results in seconds



Food and Beverage: Pomegranate Juice Adulteration

• Pomegranatejuiceisapproximately5timesmoreexpensivethangrapejuice,acommonadulterant.

• Tartaricacid,presentingrapejuiceandabsentinpomegranatejuicecanbeusedasamarkertodetectadulterationofpomegranatejuice

• Successfulmeasurementoflevelsaslowas1%grapejuiceinpomegranatejuice



TOF MS



Easy to use

Fast, accurate mass

• PropanethiolS-oxideinonionsisknowntocausetheeye’stotear(whencuttingtheonion)

• 1cm3pieceofonionwasdirectlyanalyzed

• Withnosamplepreparation,DSA/TOFanalysisoftheonionsampledetectedPropanethiolS-oxidewithhighmassaccuracy


Food and Beverage: Propanethiol S-oxide in Onions


TOF MS


Easy to use

Increased sensitivity

Rapid analysis

• Resveratrolisnaturallyoccurringpolyphenolpresentingrapeskinandseeds

• Itisanantioxidantthoughttobepresentinhigherlevelsinredwineandlinkedtomanyhealthbenefits

• DSA/TOFanalysisinTrapPulse™modeof1µLofredwine(onamesh)providestherequiredsensitivityfordetectionandconfirmationofresveratrol


Food and Beverage: Resveratrol in Red Wine


TOF MS


Easy to use

Comparison of products

Rapid analysis

• Somesterolsinoliveoilarethoughttodecreasebloodcholesterol

• Saponifiedoliveoilwasdirectlyanalyzedforsterols

• DSA/TOFanalysisdetectsthebeneficialsterolsinoliveoilwithminimalsamplepreparation

• Oliveoilscanrapidlybecomparedfordetectionofbeneficialsterols


Food and Beverage: Sterols in Olive Oil


TOF MS


Easy to use

Component analysis


• Artificialsweetenersareoftenusedindietcola

• Sweetenersindietcolawasdirectlyanalyzedwithoutanysamplepreparation

• DSA/TOFanalysisconfirmssweetenersusedindietcolaaswellasotheradditiveswithaccuratemass


Food and Beverage: Sweeteners in Diet Cola


TOF MS


Environmental: Atrazine in Water

Results in seconds

Increased sensitivity

Confirms water safety

• Thepesticideatrazineisacontaminantofsurfaceanddrinkingwater

• Themaximumlevelofatrazineinwaterhasbeensetas0.003mg/L

• UseofTrapPulse™modeincreasessensitivity8foldandgivesgreatermassaccuracy

• DSA/TOFanalysisof2µLofwateronameshconfirmspresenceofatrazinewithamassaccuracy<1ppm



TOF MS


Environmental: Carbamates in River Water

No complex method development

Fast, accurate mass

Ensures water quality

• Carbamatesareknowncontaminantsofriverwater,EPAmaximumconcentrationof10ug/L

• ExistingprotocolsrequirelengthySPEworkupfollowedbyLC,LC/MSorGC/MSanalysis

• 10ppbspikedriversamplessimplyfilteredandpipettedontoamesh

• DSA/TOFanalysisconfirmspresenceofcarbamates,withhighmassaccuracy



TOF MS


Environmental: Insecticide on Mosquito Nets

Results in seconds


Protects consumers

• DeltamethrinisaWHOapprovedinsecticidefortreatmentofmosquitonets

• Treatednetscommandahigherpricebutsomesuppliersomittheinsecticide

• ExistingprotocolsrequireextractionfollowedbyHPLCorGC/MSanalysis

• DSA/TOFanalysisofanetsectionconfirmspresenceofdeltamethrinattherequiredleveltobeeffective



TOF MS


No complex method development

Comprehensive analysis

Ensures water quality

• Personalcareproductsposearisingconcernasacontaminantinpostwatertreatmentriverwaters

• ExistingprotocolsrequirelengthySPEworkupfollowedbyLC,LC/MSorGC/MSanalysis

• 10ppbspikedriversamplessimplyfiltered,10mMammoniumformateadded,andpipettedontoamesh

• DSA/TOFanalysisconfirmspresenceofpersonalcareproductsandpesticides,withhighmassaccuracy


Environmental: Personal Care Products in River Water


TOF MS


Chemical: Bisphenol A in Plastic

Easy-to-use

No sample prep or chromatography

Protects consumers

• BisphenolA(BPA)isusedalongwithothermaterialstomakeplastics.Itischaracterizedasanendocrinedisruptormimickingnaturalhormoneswhichhaselevatedsafetyconcernsaboutitleachingintoourfoodfromthepackagingandnegativelyimpactinghumanhealth.

• In2010,theFDAwarnedofthepossiblehazardtoyoungchildrenandBPAwasbannedfrombabybottles.

• DSA/TOFdirectanalysisofasectionofplasticbottleconfirmspresenceofBPAwithaccuratemass.



TOF MS


Chemical: Ferulic Acid in Skin Oil

Rapid analysis

Protects customers


• Ferulicacidisanantioxidantoftenaddedtoanti-agingskinproducts

• Cosmeticskinoilwasanalyzedtodetermineifferulicacidwaspresent

• DSA/TOFdirectanalysisofcosmeticskinoilconfirmsthepresenceofferulicacidwithaccuratemass

• Analysiswasperformedin15secondswithnosamplepreparation


TOF MS


Easy to use

No chromatography

Fast accurate mass

Chemical: Fullerene C-60

• Buckminsterfullerenesareresearchedfortheirtechnologicalapplicationsinmaterialsscienceandnanotechnology.

• DSA/TOFanalysis,innegativemode,ofa1mg/mLfullereneC-60intoluene



TOF MS


Easy to use

Compound confirmation


• Limoneneisamoleculethatgivesorangestheirstrongsmellandisoftenusedincleaningproductsandaprecursorforchemicalsynthesis

• Samplepreparationandmethoddevelopmentforanalysisoflimoneneislengthyandtimeconsuming

• Limoneneismeasuredinorangepeelwithdirectanalysisandaccuratemassconfirmation


Chemical: Limonene in Orange Peel


TOF MS


Chemical: Methylparaben in Hair Gel

Rapid, accurate results

Protects consumers

No sample prep or method development

• Parabensareaclassofchemicalsusedinpreservationofpersonalcareproductsandareimplicatedtonegativelyimpacthumanhealth

• Traditionalsamplepreparationandmethoddevelopmentofparabensistimeconsuming

• DSA/TOFdirectanalysisofpersonalcareproductsconfirmsthepresenceofmethylparabenwithaccuratemass



TOF MS


Chemical: Paraben Screening in Texture Cream

Easy to use

Ensures product safety

No sample prep

• Parabensareaclassofchemicalsusedinpreservationofpersonalcareproductsandareimplicatedtonegativelyimpacthumanhealth

• Traditionalsamplepreparationandmethoddevelopmentofparabensistimeconsuming,approximately25minpersample

• DSA/TOFallowedforfastscreeningofparaben-freetexturecreamandconfirmedtheabsenceofparabenswithhighmassaccuracy



TOF MS


Easy to use

No chromatography

Protects consumers

• Parabensarewidelyusedinlipstickstoimproveshelflifebutlinkstobreasttumourshavebeenfound

• DSA/TOFdirectanalysisoflipstickinaglasscapillaryconfirmspresenceofparabenswithaccuratemass


Chemical: Parabens in Lipstick


TOF MS


Easy to use



• Parabensareaclassofchemicalsusedinpreservationofcosmetics

• Samplepreparationandmethoddevelopmentofparabensislengthyandtimeconsuming

• DSA/TOFdirectanalysisoflotionconfirmsparabensinlotionwithaccuratemass


Chemical: Parabens in Lotions


TOF MS


Chemical: Salicylic Acid in Foundation

Results in seconds

Product integrity


• Salicylicacidisacommoningredientinacnefightingpersonalcareproductsusedtohelpclearandpreventskinblemishes

• Liquidfoundationwasdirectlyanalyzedtodetermineifsalicylicacidwaspresent

• DSA/TOFdirectanalysisoffoundationconfirmsthepresenceofsalicylicacidwithaccuratemass



TOF MS


Forensics: Cathinones in Bath Salts

Rapid analysis


No sample prep

• Cathinonesarecommonlyfoundinstreetdrugs,suchasbathsalts

• Currently,nostandardmethodofanalysisexistsforcathinonesinbathsaltsamples

• DSA/TOFanalysisofbathsaltsconfirmedthepresenceofbutylone,α-PVP,α-MPPP,andMDPBPwithaccuratemassofparentandfragmentions



TOF MS


Rapid analysis


No method development or sample preparation

• Cathinonesarecommonlyfoundinstreetdrugs,suchasbathsalts

• Currently,nostandardmethodofanalysisisavailableforcathinones

• DSA/TOFanalysisofcathinonestandards,butylone,2-MDPV,mephedrone,andMDPBPresultedinexcellentmassaccuracyofparentandfragmentions


Forensics: CID of Cathinone Standards


TOF MS




Fast, accurate mass

• Theminimumlevelofthedaterapedrug,Gamma-HydroxyButyricAcid,whichaffectshumansis1mg/mL

• Acolasamplewasspikedwiththedrugat0.1mg/mL,10-foldlessthantheminimumdetectionlimit

• Withnosamplepreparation,DSA/TOFanalysisofthecolasampledetectedthedrugwithhighmassaccuracy


Forensics: Date Rape Drug in Cola


TOF MS


Results in seconds


Non destructive

Forensics: Ethyl Centralite

• Residueanalysisonfabricisimportantforforensicanalysisofcrimescenes.Moderngunpowdersusenitrocelluloseandnitroglyercinasbasicingredients

• 2%Dichloromethyleneinmethanolwasinfusedat10µL/minandDSA/TOFwasruninpositivemode

• DSA/TOFanalysisonfabricidentifiedgunshotresiduebyconfirmationofethylcentralitewithaccuratemass



TOF MS


Forensics: Nitroglycerin

Results in seconds


Non-destructive

• Gunshotresidueanalysisonfabricisimportantforforensicanalysisofcrimescenes.Moderngunpowdersusenitrocelluloseandnitroglyercinasbasicingredients.

• 2%Dichloromethyleneinmethanol(asadopant)wasinfusedat10µL/mintoionizenitroglycerinasachlorideadduct

• DSA/TOFanalysisonfabricidentifiedgunshotresiduebyconfirmationofnitroglyercinwithaccuratemass



TOF MS


Easy to use

Confirms compound identity

Fast, accurate mass

• Testosteroneisananabolicsteroidthatcanbeusedtoenhancephysicalperformanceinathletes

• Testosteronepowderwasdirectlyanalyzedinaglasscapillary

• Confirmationoftestosteronewasachievedinsecondswithhighmassaccuracy


Forensics: Testosterone in Steroid Powder


TOF MS



Complete component analysis

Confirms product authenticity

• Emergen-C®isadietarysupplementdesignedtosupporthealthymetabolicfunction

• Analysisinbothpositiveandnegativemodesensurescompleteproductcharacterization

• DSA/TOFanalysisofEmergen-C®powderinaglasscapillarydetectscomponentswithahighmassaccuracy

Nutraceuticals: Components of Multivitamin Powder


TOF MS



Fast accurate mass

Assures product safety

• Albuterolsulfateinhalationaerosolisintendedfororalinhalationasatreatmentforbronchospasm.Itcontainsamicrocrystallinesuspensionofalbuterolsulfateinapropellant,andnootherexcipients.

• TheactivecompoundwasmeasuredusingDSA/TOFwhichprovidedaccuratemassconfirmation


Pharmaceutical: Aerosols/Inhalers


TOF MS


Results in seconds

No chromatography


• Panadol®Extratabletsaresolubletabletswithtwoactiveingredients,paracetamolandcaffeine,designedformildtomoderatepainrelief

• DSA/TOFanalysisofatabletdirectlydetectscomponentswithahighmassaccuracy


Pharmaceutical: Components of Panadol® Extra


Results in seconds

Complete component analysis


TOF MS


• Panadol®SinusMaxisdesignedforfastandeffectivereliefofsinuscongestionandpressure



Pharmaceutical: Components of Panadol® Sinus Max


TOF MS


Results in seconds



• Paracetamolisawidelyusedoverthecounteranalgesicandantipyretic,commonlyusedforthereliefofminorachesandpains



Pharmaceutical: Paracetamol Tablets

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Mass Spec Results In Seconds With Direct Sample …€¢ Insecticide on Mosquito Nets ... •...

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