Working Group Chair Presentation Book
AOAC SPSFAM ALLERGENS DRAFT SMPR Ͳ COMMENTS on ALLERGENS SMPR FINAL
Line Numbers(If Applicable)
Item
Comment
ProposedChange(s)
Response
Chocolateshouldbeincludedintothelistofpriorityallergens.If chocolateisaknownproblemthantheapplicabilityshouldclearly statethatchocolateisnotpossibletomeasureusingthevalidated method.
Nochange. Chocolateisanoptionalmatrixtobetestedfor candidatemethodthatclaimtoworkinchocolate.
139(table 2)
1
Chocolateisanimportantmatrixforpeanut,hazelnutandmilk.
Describethevalidationofprecisioninamoreprecisewaye.g.include numberoflevelsandreplicates
Additionalreference toAppendixDandFareadded
Shouldtheprecisiondataobtainedoverthewholeanalyticalrange?Numberoflevels?
2 56Ͳ65
Nochangerecommended. Thecommentistruebutthereis notanyprohibitionagainsttheLOQ=MDL.
116(table 1)
3
BydefinitiontheanalyticalrangecanonlystartwithanLoQ.MDLonlygivesayesorno.
Aftervalidation,LCͲMS/MSmethodswillbeusedforcomparisonwithELISAresults.Ancommercial ELISAis(often)calibratedtothewholeallergenicfoodwhileLCͲMS/MSiscalibratedtopeptides.Is comparabilityestablishedviareferencematerials?(again:traceabilityofLCͲMS/MStotheseRMsis mandatory!)
Nochange. TheworkinggroupdidnotagreetotieLCͲMS/MS resultstoELISAresults.
DiscusstraceabilityandcomparabilitytoELISAresults(note:thisSMPR discussapossiblereferencemethodforcGMPcompliance!)
4
NISTSRM2387isnotpurepeanutbutamixtureofroastedpeanut,sugar,partiallyhydrogenated vegetablesoilsandsalt.SeeNISTcertificate:proteincontentisgivenbutnotpeanutcontent.
DiscusssuitabilityofthisSRMintheworkinggroupandgiveconversion factor
Nochange. That’swillbeleftuptothemethodedeveloper.
5 96
Agree.ReplaceNISTSRM1549wuth1549a.
6 92
NISTSRM1549issupersededbyNIST1549a
DeleteNISTSRM1549
WorkingGroupagreedthatallresultstobe"reportedasppm ofthetargetallergeninfoodcommodity".
Discusstraceabilityintheworkinggroupanddiscussaconversion factor
NIST8445isawholeeggpowderwithagivenproteincontent.Howshouldamethoddeveloper traceittowholeeggwithoutconversionfactor?
7 85
AddareferencetoAppendixM: ValidationProceduresfor QuantitativeFoodAllergenELISAMethods. AppendixMdoes mandatetheuseofincurredsamples. AOACpolicyallowsfor bothkindsofsamples. Methoddeveloperdiscretion.
Recovery:Whatkindofsamplesisrequired?Spikedorincurred?ForELISAincurredispreferred.
WeshouldfollowtheguidelineforELISAwhichpreferincurred
8 67
Recovery:Howshouldamethoddeveloperdeterminethisparameter?Byspikingwithreference materialsorpeptidesoradifferentmaterial.Oneshouldrememberthatitisnotallowedtousea referencematerialforcalibrationANDspiking!Ifpeptidesareusedforcalibration,howwas traceabilityestablished?
Nochangerecommended. Methoddevelopmentissuenot SMPRissue.
Discussintheworkinggroupandremembertosolvethetraceability problem
9 67
Sincereproducibilitydeterminationisonlypossiblebyacollaborativestudy,anintraͲlaboratory reproducibilityshouldbedefinedtoeasesingleͲlabvalidationsatthebeginning
Inlcudeanewclauseafterrepeatabilityanddescribethevalidationto bedone
Nochange. AllpreviousSMPRsusedRSDRandRSDr.
10 62
7
MDL:Howshouldamethoddeveloperestimatethisparameter?Byusingblankmatricesorblank matricesspikedwithreferencematerials/peptides?Howmanyreplicates?Wehaveveryclear guidelinesforallergendeterminationbyELISAͲwhynotfor“ReferencemethodsforcGMP compliance”? LoQ:Howshouldamethoddeveloperdetermineorevenestimatethisparameter?Byusing referencematerialsorpeptidesolutionsorblankmatricesorblankmatricesspikedwithreference materials/peptides?Howmanyreplicates?Wehaveveryclearguidelinesforallergen determinationbyELISAͲwhynotfor“ReferencemethodsforcGMPcompliance”?
ReferencetoAppendixM: ValidationProceduresfor QuantitativeFoodAllergenELISAMethodsaddedtoSMPR. SMPRwillalsorefertoFDAand/orEPAdefinitionforMDL.
11 50
DiscussintheworkinggroupmaybefollowELISAguidelines
ReferencetoAppendixM: ValidationProceduresfor QuantitativeFoodAllergenELISAMethodsaddedtoSMPR.
12 46
DiscussintheworkinggroupmaybefollowELISAguidelines
Line108ofversion revised torecommend"LOQ,MDL,recovery andprecision"dataforeveryclaimedmatrix.
includeasentenceforeachparameterthatexplainstheparameterͲ specificvalidation
LoQ,MDL,recoveryandprecisiondataneedtobedeterminedforeveryclaimedmatrix
13 46Ͳ69
BytakingthelatestpublishedVITALreferencedosesC18(FoodChem.Toxicol.63:9Ͳ17,2014)itis obviousthattheMDLs/LoQsintable1arenotsufficientwhenafoodisanalyzedthatisconsumed inaservicesizeofmorethan50g. LowerMDL/LoQappropriatelytothefollowingtable.Note:C19 Hazelnut:Referencedoseasprotein:0.1mg;Referencedoseasallergenicfood:0.64mg; Minimumconcentrationtobequantifiedwhenconsuming50gfood:12.8mg/kgandfor200g3.2 mg/kg.
Nochange. WorkingGroupdiscussedon3/3/2016.Thereare multipleVITALswithdifferentmaximumpermissiable concentrations. TheWorkingGroupconsensusisthatnoneof theVITALsareinternationalconcensusnstandards,anddeclined toresettheLOQsorMDLs basedonVITALmaximum permissiableconcentrations.
116(table 1)
Milk:Referencedoseasprotein:0.1mg;Referencedoseasallergenicfood:3.03mg;Minimum concentrationtobequantifiedwhenconsuming50gfood:60.6mg/kgandfor200g15.2mg/kg.
ChangeMDLs/LoQintable1accordingtotheVITALvaluesand calculationsgivenundercomments.Discussintheworkinggroup
14
Peanut:Referencedoseasprotein:0.2mg;Referencedoseasallergenicfood:0.8mg;Minimum concentrationtobequantifiedwhenconsuming50gfood:16mg/kgandfor200g4mg/kg.
Wholeegg:Referencedoseasprotein:0.03mg;Referencedoseasallergenicfood:0.25mg; Minimumconcentrationtobequantifiedwhenconsuming50gfood:4.8mg/kgandfor200g1.2 mg/kg.
Howshouldamethoddeveloperprovethattheselectedpeptidesarenot“too”specifice.g.a sequenceisusedthatisnotpresentineverycommerciallyavailablepeanutorhazelnutvariety.On theopposite,iftheselectedpeptidesarenotspecificenough,nearbotanicalrelativesaredetected whicharemaybenotallergenicorregulated(seeprunusmahalebexample).
Atminimumachapterdescribingtheknownspecificities/selectivities shouldbeprovided.(Note:Unknownoccurrenceofpeptidesthatare notfromaallergenicsourcewillalwaysoccurinthefuture,seealso prunusmahaleb)
Nochange. Theworkinggroupdidnotagree.
15
Nochange. Theworkinggroupdidnotagree.
Whataretheminimumperformancecriteriaforpeptideselection?
Includecriteriaforpeptideselectionorgivereference
16
Nochange. WorkingGroupdiscussedon3/3/2016.Thereare multipleVITALswithdifferentmaximumpermissiable concentrations. TheWorkingGroupconsensusisthatnoneof theVITALsareinternationalconcensusnstandards,anddeclined toresettheLOQsorMDLs basedonVITALmaximum permissiableconcentrations. ANDE25
VITALvaluesarebasedonamountofproteinperservicesize.Therefore,thedefinitionofthefood allergensas“foodcommodities”withoutmentioningtheproteincontentwillestablishanonͲ comparabilitybetweenresultsobtainedbyanLCͲMS/MSmethodandVITALvalues.
Includesomeguidancefortheuserorletthemethoddeveloper describehiswayofestablishingtraceabilitytoVITALvalues
17
collaborativetest:ItshouldbecriticallycheckedifAppendixDissufficientinthecasewhereLESS than8participants(and/orLCͲMS/MSmachines)areavailable.Isthisstillcollaborativeor forbiddenatall?
Nochange. AOACpolicynotaworkinggroupdecision.
discussintheworkinggroup
18 9
Changetitleto“…selectedfoodallergens."
19 3
Thetitleisunclear
changeto“…selectedfoodallergens”
Thismeansamethodcomparisonbetweentheoriginalmethod(checkedbyanERP)andthis methodtransferredtoanotherlab.Arethereanyguidelinesforthiscase?Whatistheminimum requirednumberofmeasurementstobesurethatbothmethodsarecomparable?
Nochange. Methodcomparisionisnotaverification requirement.
20 9
Includeminimumrequirementsforverification
8
Made with FlippingBook - Online catalogs