新西兰双氰胺检测方法.docx
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新西兰双氰胺检测方法.docx
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新西兰双氰胺检测方法
DeterminationofDicyandiamide,CyanuricAcidandMelamineinDairyProductsbyHighPerformanceLiquidChromatographyTandemMassSpectrometry(LC-MS/MS)
1.ConfidentialityStatement
ThismethodisthepropertyofAsureQualityLtd.andcannotbecopied,usedordistributedwithoutthewrittenpermissionoftheWellingtonLaboratoryBusinessManager.
2.SafetyandHealth
MSDsheetsofallchemicals,solventsandstandardsmustbeunderstoodbytheanalystbeforecommencingthemethod.Avoidinhalingvaporsorchemicals.Usetheassignedprotectiveclothingandequipmentatalltimes.Ensurethatyouarefamiliarwiththelocationoffireextinguishers,firstaidkitandanysafetyequipmentthatmayberequired.
RefertotheLaboratory'sHazardRegisterforSignificantHazardsidentifiedandthecontrolmethodsspecifiedtominimisethesehazards.
2.1SpecificHazardsandControlMethods
NotApplicable.
3.definitions
3.1ABBREVIATIONS
DCD
Dicyandiamide
HPLC
HighPerformanceLiquidChromatography
IR
IonRatio
IS
InternalStandard
KTP
KeyTechnicalPersonnel
LC-MS/MS
LiquidChromatographyTandemMassSpectrometry
LIMS
LaboratoryInformationManagementSystem
LOD
LimitofDetection
LOQ
Limit(orLevel)ofQuantification
LOR
LimitofReporting
M
MolecularMass
MRM
MultipleReactionMonitoring
MSDsheets
MaterialSafetyDatasheets
PVDF
PolyvinylideneFluoride
Q1
Quantificationion
Q2
Secondaryquantification(check)ion
QC
QualityControl
RR
RelativeResponse
RS
RecoveryStandard
RT
RetentionTime
SOP
StandardOperatingProcedure
U
UncertaintyofMeasurementwith95%confidenceinterval
WS
WorkingStandard
3.2DEFINITIONOFTERMS
Analyte:
Thisisthecomponentofasamplethathastobedetected,identifiedandquantified.Theterm“analyte”includes,whereappropriate,derivativesformedfromtheanalyteduringanalysis.
Analyticalsamples:
Samplesrequiredtobeanalysedquantitativelyforthepresenceoftargetanalytes.
ExternalStandard:
AsolutionintheHPLCsolventwhichhasbeenfortifiedwithknownamountsofanalytesandinternalstandard.
InternalStandard(IS):
Compoundaddedatthebeginningoftheanalysis,whichissimilartothetargetanalytesinchemicalcompositionandbehaviour.
LimitofDetection(LOD):
Thatconcentrationofanalytewhichgivesaninstrumentsignalsignificantlydifferentfromtheblank.Commonlydefinedasthemeanblanklevelplus3SDofblankmeasurements.
Limit(orLevel)ofQuantification(LOQ):
Regardedasthelowerlimitforprecisequantitativemeasurements(Commonlydefinedaseitherthemeanblanklevelplus10SDofblankmeasurementsor3LOD.Commonlyisrepresentedbythelowestconcentrationcalibrationstandard,sothatsamplescannotbequantifiedbelowthisstandard(bydefinition)).
LimitofReporting(LOR):
ThepracticallimitofresiduequantificationatorabovetheLOQ.TheLORmustbenolowerthanthelowestcalibrationstandard;alimitspecifiedbyaregulatorybodyorclient.
MatrixBlank(RecoveryBlank):
Ablankpreparedfromthesametypeasthematrixofinterest.
MatrixRecoverySample(RecoverySample):
Asamplepreparedfromthematrixblanktowhichisaddedknownamountsofanalytesandinternalstandardinordertoestablishtheefficacyofthemethod.Inthismethodtheyarealsousedascalibrationsamplestoquantifyanalytesinanalyticalsamples.
Reagentblankdetermination:
Thisisthecompleteanalyticalprocedureappliedwithomissionofthetestportionorusinganequivalentamountofsuitablesolventinplaceofthetestportion.
RelativeResponse(RR):
Ratiooftheresponseofananalytetoitsinternalstandard.
RecoveryStandard(RS):
Compoundaddedattheendoftheanalysis.
4.IntroductionandOverview
4.1INTRODUCTION
Foodcontaminantanalysisinagriculturalproductsisofvitalimportanceforthesafetyofourfoodandtosafeguardourexportmarkets.
4.2SCOPE
Themethodhasbeenvalidatedinmilkandmilkpowders.Itcanbeusedforothersimilarmatricesprovidedthatitisdemonstratedthatthemethodperformancevaluesaremet.Additionalvalidationandrecordsthatmayberequiredwillbeaccordingtotherelevantvalidationprocedureofthelaboratory.
NOTE:
Refertotherelevantvalidationprocedureforvalidationactionsrequiredifadditionalmatrices/analytestothosealreadyvalidatedarerequiredtobeusedbythemethod.
4.3METHODSUMMARY
Samplesofmilkorreconstituteddairypowderaredilutedwithacetonitrile,sodiumchlorideisaddedandaftercentrifugation,filtrationandadditionofarecoverystandardtheresultingacetonitrilesolutionisanalysedbyLC-MS/MS.
4.4ANALYTES
AnalytesandInternalStandardsaresummarisedinTable1.
TABLE1:
TestArticles(AnalytesandInternalStandards)
TestArticles
CASNumber*
Analytes
Dicyandiamide(2-cyanoguanidine)
461-58-5,M=84
CyanuricAcid
108-80-5,M=129
Melamine
108-78-1,M=126
InternalStandards
[13C315N3]Melamine(RecoveryStandard)
M=132
[13C3]Melamine
1173022-88-2,M=129
[13C3]CyanuricAcid
201996-37-4,M=132
*M=molecularmass
Structures
NotApplicable.
5.ReferencedDocuments
AM-006:
AnalyticalMethods–UnidentifiedAnalyticalResponses–InvestigationandRecordKeeping
AM-013:
Chemicals,ReagentsandSolutions
AsureQualityLimitedValidationReportVR-290,DeterminationofCyanuricAcidandMelamineinMilkandPowderedMilkproductsbyHighPerformanceLiquidChromatographyTandemMassSpectrometry(LC-MS/MS),October2008
AsureQualityLimitedValidationReportVR-441,DeterminationofDicyandiamide,CyanuricAcidandMelamineinMilkandPowderedMilkproductsbyHighPerformanceLiquidChromatographyTandemMassSpectrometry(LC-MS/MS),May2010
AsureQualityLimitedValidationReportVR-499,DeterminationofCyanuricAcidandMelamineinMilkandPowderedMilkproductsbyHighPerformanceLiquidChromatographyTandemMassSpectrometry(LC-MS/MS).SupplementaryvalidationtoVR-290,January2011
EQ-004:
WorkingStandards–Preparation,CheckingandRecords
EQ-043:
EquipmentProcedureforLC-MS/MS
EQ-058:
PrimaryStandards–Ordering,StorageandRecords
QC-025:
UncertaintyofMeasurementinAnalyticalResults
QC-026:
ControlChartsProcedure
QC-028:
QualityControl–BlindSpike/Intra-LaboratoryCheckSampleScheme
QC-029:
QualityControlProceduresforAnalyticalResults
SR-012:
SamplePreparation
6.Reagents
RefertoAM-013.
DONOTUSEEXPIREDCHEMICALS,REAGENTSORSOLUTIONS.
Allreagentsandchemicalsmustbeofsuchagradethattheydonotinterferewiththeanalyticalprocess.Usethestatedgradeorequivalent.
6.1CHEMICALS
∙Aceticacid(analyticalgrade)
∙Acetonitrile,(pesticidegrade)
∙Ammoniumacetate(analyticalgrade)
∙Deionisedwater
∙Dichloromethane(analyticalgrade)
∙Sodiumchloride(analyticalgrade)
6.2SOLUTIONS
∙HPLCSolventA
Intoa1000mLSchottbottleadd0.77gofammoniumacetateand1000mLofdeionisedwater.Stiruntilthesolidisdissolved.
Storeatroomtemperature.Stablefor2weeks.
∙HPLCSolventB
Intoa2000mLSchottbottleadd1.54gofammoniumacetateand60mLofdeionisedwater.Stiruntilthesolidisdissolved.Usinga2000mLmeasuringcylinder,add1940mLofacetonitrile.Warmthebottletoapproximately50oC(waterbath)toaidcompletedissolutionofammoniumacetate.
Storeatroomtemperature.Stablefor2weeks.
7.STANDARDS
RefertoSOPsEQ-004andEQ-058.
Uponreceipt,anorange“WaitingApproval”labelisplacedonthestandard.OncethestandardhasbeenfoundtobeacceptableasdeterminedinEQ-058,theorangelabelisoverlaidbyagreen“QCReleased”label,datedandinitialled.
NOTE:
Donotuseexpiredprimarystandardsorstandardsolutions.Donotusestandardswhichhavenotbeenreleased/approvedforusebyaSeniorScientist,Scientist(approvedbytheTechnicalManager)ortheTechnicalManager.
7.1PRIMARYSTANDARDS
∙MelamineisavailablefromAcrosOrganics,>99%.Cataloguenumber22048
∙CyanuricacidisavailablefromAldrich98%.Cataloguenumber185809-25G
∙DicyandiamideisavailablefromAldrich,99%.Cataloguenumber76609
∙[13C315N3]Melamine(RecoveryStandard)isavailablefromCambridgeIsotopeLaboratories,100µg/mLinwater.CataloguenumberCNLM-8150-1.2
∙[13C3]Melamine(InternalStandard)VETRANAL,10mgisavailablefromSigma-Aldrich.Cataloguenumber32666-10MG.
∙[13C3]CyanuricAcid(InternalStandard):
VETRANAL,10mg,isavailablefromSigma-Aldrich.Cataloguenumber32679-10MG,
7.2SECONDARYSTANDARDS
7.2.1UnlabelledMelamineandCyanuricAcidStandards(100µg/mL)
Weighaccurately10.0mgofstandardintoa125mLpolypropylenebottleandadd
100gofdeionisedwaterbyweighttogivea100µg/mLsolution.Capandshakethoroughlytodissolvethecompound.
Storeatroomtemperature.Solutionsarestablefortwoyears.
7.2.2DicyandiamideStandard(1mg/mL)
Weighaccurately10.0mgofstandardintoa10mLcalibratedvolumetricflask.Adddeionisedwater,shaketodissolveandmakeuptovolume.Transfertoa20mLscrewcapvialandcaptightly.
Storeatroomtemperatureinthedark.Solutionisstableforsixmonths.
7.2.3RecoveryStandard(1µg/mL)
Remove1.2mLoftheprimarystandardsolutionof[13C315N3]melaminewithacalibratedHamiltonsyringeanddiluteto120mLina125mLpolypropylenepottlewithwatertogivea1µg/mLsolution.
Secondarystandardshaveanexpirydateoftwoyearsfromthedateofpreparationofsolutionortheexpirydateoftheprimarystandard,whicheverisearlier.Thesestandardsaretobestoredatroomtemperature.
7.2.4InternalStandards(100µg/mL)
Weighaccurately10.0mgofstandardintoa125mLpolypropylenebottleandadd
100gofdeionisedwaterbyweight
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