2/MonographsAcesulfamePotassiumAcesulfameK;6-Methyl-1,2,3-oxathiazine-4(3H)-one-2,2DioxidePotassiumSaltH3COSO2NKOC4H4KNO4SFormulawt201.24INS:950CAS:[55589-62-3]DESCRIPTIONAcesulfamePotassiumoccursasawhite,free-flowingcrystal-linepowder.Itisfreelysolubleinwaterandveryslightlysolubleinethanol.FunctionNonnutritivesweetener;flavorenhancer.REQUIREMENTSIdentificationA.AddafewdropsofsodiumcobaltinitriteTStoasolutionof0.3gofsamplein1mLofglacialaceticacidand5mLofwater.Ayellowprecipitateforms.B.Dissolve10mgofsamplein1000mLofwater.Thesolutionshowsanabsorptionmaximumat227Ϯ2nm.AssayNotlessthan99.0%andnotmorethan101.0%ofC4H4KNO4Safterdrying.9FluorideNotmorethan3mg/kg.LeadNotmorethan1mg/kg.LossonDryingNotmorethan1.0%.OrganicImpuritiesNotmorethan20g/gofUV-activecompounds.pHofa1:100SolutionBetween5.5and7.5.TESTSAssayDissolvebetween200and300mgofsample,pre-viouslydriedat105°for2handaccuratelyweighed,in50mLofglacialaceticacidcontainedina250-mLflask.Note:Dissolutionmaybeslow.Add2or3dropsofcrystalvioletTStotheflask,andtitratewith0.1Nperchloricacidtoablue-greenendpointthatpersistsforatleast30s.Caution:Handleperchloricacidinanappropriatefumehood.Performablankdetermination(seeGeneralProvisions),andmakeanynecessarycorrection.Eachmilliliterof0.1Nper-chloricacidisequivalentto20.12mgofC4H4KNO4S.FluorideDetermineasdirectedinMethodIIIunderFluo-rideLimitTest,AppendixIIIB,usinga4-gsample.LeadDetermineasdirectedunderLeadLimitTest,Appen-dixIIIB,usingasolutionof2gofsamplein20mLofwater,and2goflead(Pb)ioninthecontrol.LossonDryingDetermineasdirectedunderLossonDry-ing,AppendixIIC,dryingasampleat105°for2h.OrganicImpuritiesReferenceStandard4-Hydroxybenzoicacidethylester.SampleSolutionAsolutionof10gofsampleperliterofdeionizedwater.10/AceticAcid,Glacial/Monographs食界论坛http://www.sinofood.com.cn/bbs.htm
FCCVProcedure(SeeChromatography,AppendixIIA.)Useahigh-performanceliquidchromatographcapableofseparatingacesulfamepotassiumand4-hydroxybenzoicacidethylesterwitharesolutionof2.UseachromatographequippedwithaUVordiodearray(227nm)detectoranda25-cm×4.6-mm(id)stainlesssteelcolumn,orequivalent,packedwith3to5mofreversedphaseC18silicagel,orequivalent.Theelutionisisocratic.Usea40:60(v/v)solutionofacetoni-trile:0.01M/Ltetrabutylammoniumhydrogensulfate(TBAHS)inwaterasthemobilephase,withaflowrateofabout1mL/min.Inject20LofSampleSolutionintothechromatograph,andobtainthechromatogram.Ifpeaksotherthanthatcausedbyacesulfamepotassiumappearwithinthreetimestheelutiontimeofacesulfamepotassium,carryoutasecondrunusing20LofSampleSolutiondilutedto0.2mg/L.Thesumoftheareasofallpeakselutedinthefirstrunwithinthreetimestheelutiontimeofacesulfamepotassium,exceptfortheacesulfamepotassiumpeak,doesnotexceedthepeakareaofacesulfamepotassiuminthesecondrun.pHofa1:100SolutionDetermineasdirectedunderpHDetermination,AppendixIIB.PackagingandStorageStoreinwell-closedcontainersinacool,dryplace.AceticAcid,GlacialOH3COHC2H4O2Formulawt60.05INS:260CAS:[64-19-7]FEMA:2006DESCRIPTIONAceticAcid,Glacial,occursasaclear,colorlessliquid.Itboilsatabout118°.Whenwelldilutedwithwater(e.g.,1:100),ithasavinegarodorandtaste.Itismisciblewithwater,withalcohol,andwithglycerin.FunctionAcidifier;flavoringagent.REQUIREMENTSIdentificationA1:3aqueoussolutiongivespositivetestsforAcetate,AppendixIIIA.AssayNotlessthan99.5%andnotmorethan100.5%,byweight,ofC2H4O2.LeadNotmorethan0.5mg/kg.NonvolatileResidueNotmorethan0.005%.ReadilyOxidizableSubstancesPassestest.SolidificationPointNotcoolerthan15.6°.TESTSAssayTransferabout2mLofsampleintoatared,glass-stopperedflask,andaccuratelyweigh.Add40mLofwater,thenaddphenolphthaleinTS,andtitratewith1Nsodiumhydroxide.Eachmilliliterof1Nsodiumhydroxideisequiva-lentto60.05mgofC2H4O2.LeadDetermineasdirectedforMethodIintheAtomicAbsorptionSpectrophotometricGraphiteFurnaceMethodun-derLeadLimitTest,AppendixIIIB.NonvolatileResidueEvaporate19mL(20g)ofsample,accuratelymeasured,inatareddishonasteambath,anddryat105°for1h.ReadilyOxidizableSubstancesDilute2mLofsampleinaglass-stopperedcontainerwith10mLofwater,andadd0.1mLof0.1Npotassiumpermanganate.Thepinkcolordoesnotchangetobrownwithin2h.SolidificationPointDetermineasdirectedunderSolidifica-tionPoint,AppendixIIB.PackagingandStorageStoreintightlyclosedcontainers.Acetone2-Propanone;DimethylKetoneCH3COCH3C3H6OFormulawt58.08CAS:[67-64-1]DESCRIPTIONAcetoneoccursasaclear,colorless,volatileliquid.Itismisciblewithwater,withalcohol,withether,withchloroform,andwithmostvolatileoils.Caution:Acetoneishighlyflammable.FunctionExtractionsolvent.REQUIREMENTSIdentificationMix0.1mLofsamplewith10mLofwater,add5mLof1Nsodiumhydroxide,warm,andadd5mLofiodineTS.Ayellowprecipitateofiodoformforms.AssayNotlessthan99.5%andnotmorethan100.5%ofC3H6O,byweight.Acidity(asaceticacid)Notmorethan0.002%.Aldehydes(asformaldehyde)Notmorethan0.002%.Alkalinity(asammonia)Notmorethan10mg/kg.DistillationRangeWithinarangeof1°,including56.1°.FCCVMonographs/AcetonePeroxides/11食界论坛http://www.sinofood.com.cn/bbs.htm
LeadNotmorethan1mg/kg.MethanolNotmorethan0.05%.NonvolatileResidueNotmorethan10mg/kg.PhenolsPassestest.RefractiveIndexBetween1.358and1.360.SolubilityinWaterPassestest.SpecificGravityNotgreaterthan0.7880at25°/25°(equiv-alentto0.7930at20°/20°).SubstancesReducingPermanganatePassestest.WaterNotmorethan0.5%.TESTSAssayTransferabout1gofsample,accuratelyweighed,intoa1000-mLflaskcontaining20mLofwater,anddilutetovolumewithwater.Place10mLofthissolutionintoaglass-stopperedflask,add25mLofsodiumhydroxideTS,andallowthemixturetostandfor5min.Add25mLof0.1Niodine,stoppertheflask,allowthecontentstostandinacold,darkplacefor10min,andadd30mLof1Nsulfuricacid.Titratetheexcessiodinewith0.1Nsodiumthiosulfate,usingstarchTSastheindicator.Performablankdetermination(seeGeneralProvisions),andmakeanynecessarycorrection.Eachmilliliterof0.1Niodineisequivalentto0.9675mgofC3H6O.Acidity(asaceticacid)Mix38mLofsamplewithanequalvolumeofcarbondioxide-freewater,add0.1mLofphenol-phthaleinTS,andtitratewith0.1Nsodiumhydroxide.Notmorethan0.1mLisrequiredtoproduceapinkcolor.Aldehydes(asformaldehyde)PrepareaSampleSolutionbydiluting2.5mLofsamplewith7.5mLofwater.PrepareaStandardSolutioncontaining40gofformaldehydein10mLofwater.Add0.15mLofa5%solutionof5,5-dimethyl-1,3-cyclohexanedioneinalcoholtoeachsolution,andevapo-rateonasteambathuntiltheAcetoneisvolatilized.Diluteto10mLwithwater,andcoolquicklyinanicebathwhilestirringvigorously.AnyturbidityproducedintheSampleSolutiondoesnotexceedthatproducedintheStandardSo-lution.Alkalinity(asammonia)Add1dropofmethylredTSto25mLofwater,add0.1Nsulfuricaciduntilaredcolorjustappears,thenadd23mLofsample,andmix.Notmorethan0.1mLof0.1Nsulfuricacidisrequiredtorestoretheredcolor.DistillationRangeDetermineasdirectedunderDistillationRange,AppendixIIB.LeadDetermineasdirectedforMethodIintheAtomicAbsorptionSpectrophotometricGraphiteFurnaceMethodun-derLeadLimitTest,AppendixIIIB.MethanolPrepareaSampleSolutionbydiluting10mLofsampleto100mLwithwater.PrepareaStandardSolutioninwatercontaining40gofmethanolineachmilliliter.Add0.2mLof10%phosphoricacidand0.25mLof1:20potassiumpermanganatesolutionto1mLofeachsolution.Allowthemixturestostandfor15min,thenadd0.3mLof1:10sodiumbisulfitesolutiontoeach,andshakeuntilcolorless.Slowlyadd5mLofice-cold80%sulfuricacid,keepingthemixturescoldduringtheaddition.Add0.1mLof1:100chromotropicacidsolution,mix,anddigestonasteambathfor20min.AnyvioletcolorproducedintheSampleSolutiondoesnotexceedthatproducedintheStandardSolution.NonvolatileResidueEvaporate125mL(about100g)ofsampletodrynessinatareddishonasteambath,drytheresidueat105°for30min,cool,andweigh.PhenolsEvaporate3mLofsampletodrynessat60°.Add3dropsofasolutionof100mgofsodiumnitritein5mLofsulfuricacidtotheresidue,allowthemixturetostandforabout3min,andthencarefullyadd3mLof2Nsodiumhydroxide.Nocolorappears.RefractiveIndexDetermineasdirectedunderRefractiveIndex,AppendixIIB,usinganAbbe´orotherrefractometerofequalorgreateraccuracy.SolubilityinWaterMix38mLofsamplewithanequalvolumeofcarbondioxide-freewater.Thesolutionremainsclearforatleast30min.SpecificGravityDeterminebyanyreliablemethod(seeGeneralProvisions).SubstancesReducingPermanganateTransfer10mLofsampleintoaglass-stopperedcylinder,add0.05mLof0.1Npotassiumpermanganate,mix,andallowtostandfor15min.Thepinkcolordoesnotentirelydisappear.WaterDetermineasdirectedunderWaterDetermination,AppendixIIB,usingfreshlydistilledpyridineinsteadofmeth-anolasthesolvent.PackagingandStorageStoreintightcontainersremotefromfire.AcetonePeroxidesINS:929CAS:[1336-17-0]DESCRIPTIONAcetonePeroxides,usuallymixedwithanediblecarriersuchascornstarch,occurasafine,white,free-flowingpowder.Theyareamixtureofmonomericandlineardimericacetoneperoxides(mainly2,2-hydroperoxypropane),withminorpro-portionsofhigherpolymers.Caution:AcetonePeroxidesarestrongoxidizingagents.Avoidexposuretotheskinandeyes.FunctionBleachingagent;maturingagent;doughcondi-tioner.REQUIREMENTSIdentificationDissolveabout20mgofsamplein5mLof1:10sulfuricacid,allowtostandforafewminutes,andaddadropofpotassiumpermanganateTS.Thepinkcolordisappears.AssayAsampleyieldsanamountofhydrogenperoxideequivalenttonotlessthan16.0%ofAcetonePeroxides.LeadNotmorethan4mg/kg.12/AcetylatedMonoglycerides/Monographs食界论坛http://www.sinofood.com.cn/bbs.htm
FCCVTESTSAssayTransferabout200mgofsample,accuratelyweighed,intoa250-mLbeaker,add50mLof1:10sulfuricacid,allowtostandforatleast3min,stirringoccasionally,andtitratewith0.1Npotassiumpermanganatetoalightpinkcolorthatpersistsforatleast20s.Calculatethetotalperox-ides,P,asgramsofhydrogenperoxideequivalentsper100gofthesample,bytheequationP=V×N×0.017×100/W,inwhichVandNarethevolumeandexactnormality,respec-tively,ofthepotassiumpermanganate;0.017isthemilliequi-valentweightofhydrogenperoxide;andWistheweight,ingrams,ofthesampletaken.MultiplythevaluePsoobtainedby1.6toconverttopercentAcetonePeroxides.LeadDetermineasdirectedunderLeadLimitTest,Appen-dixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds,and4goflead(Pb)ioninthecontrol.PackagingandStorageStoreintightlyclosedcontainersinacool,dryplace,preferablybelow24°.AcetylatedMonoglyceridesAcetylatedMono-andDiglycerides;AceticandFattyAcidEstersofGlycerol;AcetoglyceridesCH2OR1CHOR2CHOR3in which R1, R2, and R, or H. At least one R must be a 3 each may be a fatty acid moiety, COCHfatty acid, and at least one must be COCH33.INS:472aDESCRIPTIONAcetylatedMonoglyceridesoccurasclear,thinliquidsorsolids,rangingincolorfromwhitetopaleyellow.Theyconsistofpartialorcompleteestersofglycerinwithamixtureofaceticacidandediblefat-formingfattyacids.Theymaybemanufacturedbytheinteresterificationofediblefatswithtriacetinandglycerininthepresenceofcatalyticagents,fol-lowedbymoleculardistillation,orbythedirectacetylationofediblemonoglycerideswithaceticanhydrideandwithouttheuseofacatalystormoleculardistillation.Theyareinsolu-bleinwater,butaresolubleinalcohol,inacetone,andinotherorganicsolvents,theextentofsolubilitydependingonthedegreeofesterificationandthemeltingrange.FunctionEmulsifier;coatingagent;texture-modifyingagent;solvent;lubricant.REQUIREMENTSAcidValueNotmorethan6.LeadNotmorethan2mg/kg.Reichert-MeisslValueBetween75and200.Thefollowingspecificationsshouldconformtotherepresenta-tionsofthevendor:FreeGlycerin,IodineValue,andSaponifi-cationValue.TESTSAcidValueDetermineasdirectedinMethodIIunderAcidValue,AppendixVII.FreeGlycerinDetermineasdirectedunderFreeGlycerinorPropyleneGlycol,AppendixVII.IodineValueDetermineasdirectedunderIodineValue,AppendixVII.LeadDetermineasdirectedintheFlameAtomicAbsorptionSpectrophotometricMethodunderLeadLimitTest,AppendixIIIB,usinga10-gsample.Reichert-MeisslValueDetermineasdirectedunderReichert-MeisslValue,AppendixVII.SaponificationValueDetermineasdirectedunderSaponi-ficationValue,AppendixVII.PackagingandStorageStoreinwell-closedcontainers.N-Acetyl-L-MethionineN-Acetyl-L-2-amino-4-(methylthio)butyricAcidCH3SCH2CH2CHCOOHHNCOCH3C7H13NO3SFormulawt191.25CAS:[65-82-7]View IRDESCRIPTIONN-Acetyl-L-Methionineoccursasacolorlessorlustrous,white,crystallinesolidorawhitepowder.Itissolubleinwater,inalcohol,inalkalisolutions,andindilutemineralacids,butpracticallyinsolubleinether.FunctionNutrient.REQUIREMENTSIdentificationTheinfraredabsorptionspectrumofthesam-pleexhibitsrelativemaximaatthesamewavelengthsasthoseFCCVMonographs/AcidHydrolysatesofProteins/13食界论坛http://www.sinofood.com.cn/bbs.htm
ofatypicalspectrumasshowninthesectiononInfraredSpectra,usingthesametestconditionsasspecifiedtherein.AssayNotlessthan98.5%andnotmorethan101.5%ofC7H13NO3S,calculatedonthedriedbasis.LeadNotmorethan5mg/kg.LossonDryingNotmorethan0.5%.Optical(Specific)Rotation[␣]D20°:Between–18.0°and–22.0°afterdrying.ResidueonIgnitionNotmorethan0.1%.TESTSAssayTransferabout250mgofthesample,accuratelyweighed,intoaglass-stopperedflask,andadd100mLofwater,5gofdibasicpotassiumphosphate,2gofmonobasicpotassiumphosphate,and2gofpotassiumiodide.Mixwelltodissolve,add50.0mLof0.1Niodine,stoppertheflask,andmix.Allowtostandfor30min,addstarchTSindicator,andthentitratetheexcessiodinewith0.1Nsodiumthiosulfate.Performaresidualblanktitration.Eachmilliliterof0.1Niodineisequivalentto9.563mgofC7H13NO3S.LeadDetermineasdirectedunderLeadLimitTest,Appen-dixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds,and5goflead(Pb)ioninthecontrol.LossonDryingDryat105°for2h.Optical(Specific)RotationDetermineasdirectedunderOptical(Specific)Rotation,AppendixIIB,usingasolutioncontaining2gofthepreviouslydriedsampleinsufficientwatertomake100mL.ResidueonIgnitionIgnite1gasdirectedinMethodIunderResidueonIgnition(SulfatedAsh),AppendixIIC.PackagingandStorageStoreintightlyclosed,light-resis-tantcontainers.AcidHydrolysatesofProteinsAcid-HydrolyzedProteins;HydrolyzedVegetableProtein(HVP);HydrolyzedPlantProtein(HPP);Hydrolyzed(Source)ProteinExtract;Acid-HydrolyzedMilkProteinDESCRIPTIONAcidHydrolysatesofProteinsoccurasliquids,pastes,pow-ders,orgranules.Theyarecomposedprimarilyofaminoacids,smallpeptides(peptidechainsoffiveorfeweraminoacids),andsaltsresultingfromtheessentiallycompletehydro-lysisofpeptidebondsinedibleproteinaceousmaterials,cata-lyzedbyfood-gradeacidsand/orheat.Cleavageofpeptidebondstypicallyrangesfromalowof85%toessentially100%.Inprocessing,theproteinhydrolysatesmaybetreatedwithsafeandsuitablealkalinematerials.Theedibleproteinaceousmaterialsusedasrawmaterialsarederivedfromcorn,soy,wheat,yeast,peanuts,rice,orothersafeandsuitablevegetableorplantsources,orfrommilk.FunctionFlavoringagent;flavorenhancer.REQUIREMENTSNote:Performallcalculationsonthedriedbasis.Evap-orateliquidandpastesamplestodrynessinasuitabletaredcontainer;then,asforthepowderedandgranularforms,drytoconstantweightat105°(seeGeneralProvisions).Assay(TotalNitrogen;TN)Notlessthan4.0%.␣␣-AminoNitrogenNot-AminolessthanNitrogen/Total(AN)62.0%andnotNitrogenNotlessmorethan(AN/TN)than3.0%.85.0%whenPercentcalculatedRatioonanammonianitrogen-freebasis.AmmoniaNitrogen(NH3-N)Notmorethan1.5%.3-Chloropropane-1,2-diol(3-CPD)Notmorethan1mg/kg.1,3-Dichloro-2-propanol(DCP)Notmorethan0.05mg/kg.GlutamicAcidNotmorethan20.0%asglutamicacid(C5H9NO4)andnotmorethan35.0%ofthetotalaminoacids.InsolubleMatterNotmorethan0.5%.LeadNotmorethan3mg/kg.PotassiumNotmorethan30.0%.SodiumNotmorethan20.0%.TESTSAssay(TotalNitrogen;TN)DetermineasdirectedunderNitrogenDetermination,AppendixIIIC.␣Amino-AminoNitrogenNitrogenDetermination(AN)Determine,AppendixasdirectedIIIC.under␣-␣Calculate-AminoNitrogen/TotalbydividingtheNitrogenpercentof(AN/TN)␣-aminoPercentnitrogenRatio(AN)bythepercentoftotalnitrogen(TN)ascorrectedforammonianitrogen(NH3-N)accordingtotheformula100[(AN−NH3-N)/(TN−NH3-N)].AmmoniaNitrogen(NH3-N)DetermineasdirectedunderAmmoniaNitrogen,AppendixIIIC.3-Chloropropane-1,2-diol(3-CPD)3-CPDStockSolutionTransfer12.5mgofreagent-grade3-chloropropane-1,2-diol(3-CPD),accuratelyweighed,intoa100-mLvolumetricflask,dilutetovolumewithethylacetate,andmix.Dilute3-CPDSolutionDilute5mLof3-CPDStockSolu-tionto100mLwithethylacetatetoyieldasolutioncontaining6.25g/mLof3-CPD.InternalStandardSolutionTransfer50mgof1-chlorote-tradecaneintoa50-mLvolumetricflask,anddilutetovolumewithethylacetate.Dilute1mLofthissolutionto100mLwithethylacetatetoyieldasolutioncontaining10g/mLof1-chlorotetradecane.StandardSolutionsA.Pipet2mLofDilute3-CPDSolutionand2.5mLofInternalStandardSolutionintoa25-mLvolumetricflask,14/AcidHydrolysatesofProteins/Monographs食界论坛http://www.sinofood.com.cn/bbs.htm
FCCVdilutetovolumewithethylacetate,andmix.TheresultingStandardSolutionAcontains0.5g/mLof3-CPD.B.Pipet8mLofDilute3-CPDSolutionand2.5mLofInternalStandardSolutionintoa25-mLvolumetricflask,dilutetovolumewithethylacetate,andmix.TheresultingStandardSolutionBcontains2.0g/mLof3-CPD.C.Pipet16mLofDilute3-CPDSolutionand2.5mLofInternalStandardSolutionintoa25-mLvolumetricflask,dilutetovolumewithethylacetate,andmix.TheresultingStandardSolutionCcontains4.0g/mLof3-CPD.Procedure(SeeChromatography,AppendixIIA)Useagaschromatographequippedwithanelectrolyticconductivitydetectoroperatedinthehalogenmodeandfittedeitherwithacapillaryinjectoroperatedinthesplitlessmodeorwithapurged,packedinjectorwithaglassinsert.Usea30-m×0.53-mm(id),fused-silicacolumn,orequivalent,coatedwith1-mSupelcowax10oranequivalentbondedcarbowaxcol-umnfittedwitha50-cmretentiongapof0.53-mm,deacti-vated,fusedsilica,orequivalent.Setthecolumntemperatureto170°for5min,raisethetemperatureatarateof5°/minto250°,andholditatthattemperaturefor10min.Maintaintheinjectortemperatureat225°.Useheliumasthecarriergasataflowrateof8mL/min.Usehydrogenasthereactantgasataflowrateof30mL/min,anduse1-propanolasthesolventataflowratethroughthecellof0.5mL/minoratthemanufacturer’sspecifiedflowratefortheoptimumoperationoftheelectrolyticconductivitydetector.Thereactortemperatureshouldbe900°,withabasetemperatureof275°.Minimizecontaminationofthereactiontubebyventingflowfromthecolumnatalltimes,exceptforthetimeduringwhichcompoundsofinterestelute.Inject1LofeachStandardSolutionA,B,andC,intothegaschromatograph.Calculatetheresponsearearatiosof3-CPDtotheInternalStandardSolutionforeachStandardSolution.Plottheresponsearearatiosversusthemicrogramsof3-CPDineachStandardSolutiontoobtainthestandardcurve.Adjustanaccuratelyweighedsample,asneeded,with20%aqueoussodiumchloridetoobtainaSampleSolutionwithasolidscontentof36%.Transfera20-galiquotoftheSampleSolutionintoa20-mLExtrelutNTcolumn(EMScience,Gibbstown,NJ),orequivalent,andallowittoequilibratefor15min.Elutethecolumnwith150mLofethylacetate,collectingtheeluentina250-mLshort-neck,round-bottomflaskwitha24/40joint.Usingarotaryevaporatorat50°,concentratetheeluenttoavolumeofapproximately3mL.Add0.5mLofInternalStandardSolutiontotheeluent,transferthismixturetoa4-dramscrew-capvial,anddilutetoavolumeof5.0mL.Inject1Lintothegaschromatograph,measureitsresponsearearatioof3-CPDtotheInternalStandardSolution,anddeterminefromthestandardcurvethemicrogramsof3-CPDinthe20-galiquottaken.1,3-Dichloro-2-propanol(DCP)EluentTransfer850mLofchromatographic-gradepen-taneand150mLofchromatographic-gradediethyletherintoasuitablecontainer,andmixwell.DCPStockSolutionTransfer50mgofreagent-grade1,3-dichloro-2-propanol(DCP),accuratelyweighed,intoa50-mLvolumetricflask,dilutetovolumewithEluent,andmix.DiluteDCPSolutionStepwiseandquantitativelydilutetheDCPStockSolutionwithEluenttoobtainafinalsolutioncontaining1g/mLofDCP.InternalStandardSolutionTransfer50mgoftrichloro-benzeneintoa50-mLvolumetricflask,dilutetovolumewithEluent,andmix.Usea1:1000dilutionofthissolutionastheInternalStandardSolution.StandardSolutionsPipet1-,2-,3-,and4-mLportionsofDiluteDCPSolutionintoseparate50-mLvolumetricflasks.Add1.0mLofInternalStandardSolutiontoeach,dilutetovolumewithEluent,andmix.SamplePreparationDissolve5.0gofsample,accuratelyweighed,inaminimalvolumeof20%aqueoussodiumchlo-ridesolution.QuantitativelytransferthissolutiontoanEx-trelutNTcolumn(EMScience,Gibbstown,NJ),orequivalent.After15min,elutethecolumnwiththree20-mLportionsofEluent,andcollectalltheeluate.Carefullyevaporatetheeluatetolessthan4mL.Add1.0mLofInternalStandardSolution,anddilutewithEluent,asnecessary,tobringthefinalvolumeto5.0mL.Procedure(SeeChromatography,AppendixIIA)Useagaschromatographequippedwithasplitinjectorandanelec-tron-capturedetectorandfittedwitha50-m×0.2-mm(id),fused-silicacolumn(Carbowax20M,orequivalent)coatedwithdimethylpolysiloxane,orequivalent.Usenitrogenasthecarriergasataflowrateof8mL/min.Beforeuse,preconditionthecolumnbyheatingitat200°andthedetectorat300°for24h.Settheinjectortemperatureat250°andtheelectron-capturedetectorat300°,andprogramthecolumntemperatureasfollows:Maintainfor10minat115°,raiserapidlyat30°/minto200°,andmaintainat200°for12min.Inject1.0LofeachofthefourStandardSolutionsintothegaschromatograph.ForeachStandardSolution,calculatetheresponsearearatiosofDCPtotheInternalStandardSolution.PlottheresponsearearatiosversusthemicrogramsofDCPineachStandardSolutiontoobtainthestandardcurve.Similarly,inject1.0LofSamplePreparation.Measureitsresponseratio,anddeterminefromthestandardcurvethemicrogramsofDCPinthesampletaken.GlutamicAcidDetermineasdirectedunderGlutamicAcid,AppendixIIIC.InsolubleMatterTransferabout5gofsample,accuratelyweighed,intoa250-mLErlenmeyerflask,add75mLofwater,covertheflaskwithawatchglass,andboilgentlyfor2min.Filterthesolutionthroughataredfilteringcrucible,dryat105°for1h,cool,andweigh.LeadDetermineasdirectedunderLeadLimitTest,Appen-dixIIIBusingaSampleSolutionpreparedasdirectedfororganiccompounds,and3goflead(Pb)ioninthecontrol.PotassiumStandardSolutionTransfer38.20mgofreagent-gradepotassiumchloride,accuratelyweighed,intoa100-mLvolu-metricflask,dissolveinanddilutetovolumewithdeionizedwater,andmix.Transfer5.0mLofthissolutionintoa1000-FCCVMonographs/AcidifiedSodiumChloriteSolutions/15食界论坛http://www.sinofood.com.cn/bbs.htm
mLvolumetricflask,dilutetovolumewithdeionizedwater,andmix.Eachmillilitercontains1.0gofpotassium(K).SampleSolutionTransfer1.00Ϯ0.05gofpreviouslydriedsample,accuratelyweighed,intoasilicaorporcelaindish.Ashinamufflefurnaceat550°for2to4h.Allowtheashtocool,anddissolvein5mLof20%hydrochloricacid,warmingthesolutionifnecessarytocompletesolutionoftheresidue.Filterthesolutionthroughacid-washedfilterpaperintoa1000-mLvolumetricflask.Washthefilterpaperwithhotwater,dilutetovolume,andmix.Usea1:300aqueousdilutionastheSampleSolution.SpectrophotometerUseanysuitableatomicabsorptionspectrophotometer.ProcedureDeterminetheabsorbanceofeachsolutionat766.5nm,followingthemanufacturer’sinstructionsforopti-mumoperationofthespectrophotometer.TheabsorbanceoftheSampleSolutiondoesnotexceedthatoftheStandardSolution.SodiumStandardSolutionTransfer25.42mgofreagent-gradesodiumchloride,accuratelyweighed,intoa100-mLvolumet-ricflask,dissolveinanddilutetovolumewithdeionizedwater,andmix.Transfer5.0mLofthissolutionintoa1000-mLvolumetricflask,dilutetovolumewithdeionizedwater,andmix.EachmilliliterofthefinalStandardSolutioncontains0.5gofsodium(Na).Preparea1:100aqueousdilutionofthissolutiontoobtainthefinalworkingStandardSolution.SampleSolutionTransfer1.00Ϯ0.05gofpreviouslydriedsample,accuratelyweighed,intoasilicaorporcelaindish.Ashinamufflefurnaceat550°for2to4h.Allowtheashtocool,anddissolvein5mLof20%hydrochloricacid,warmingthesolutionifnecessarytocompletesolutionoftheresidue.Filterthesolutionthroughacid-washedfilterpaperintoa100-mLvolumetricflask.Washthefilterpaperwithhotwater,dilutetovolume,andmix.Preparea1:4000aqueousdilutionofthissolutiontoobtainthefinalSampleSolution.SpectrophotometerUseanysuitableatomicabsorptionspectrophotometer.ProcedureDeterminetheabsorbanceofeachsolutionat589.0nm,followingthemanufacturer’sinstructionsforopti-mumoperationofthespectrophotometer.TheabsorbanceoftheSampleSolutiondoesnotexceedthatoftheStandardSolution.PackagingandStorageStoreinwell-closedcontainers.AcidifiedSodiumChloriteSolutionsDESCRIPTIONAcidifiedSodiumChlorite(ASC)Solutionsoccurasclear,colorlesstopale-yellowliquids.TheASCSolutionsareequi-libriummixturesofsodiumchlorite(NaClO2)andchlorousacid(HClO2).ASCSolutionsareproducedbyloweringthepHofasodiumchloritesolutionwithasafeandsuitableacidtoachieveapHwithintherange2.3to3.9dependingontheintendeduse.FunctionAntimicrobialagentinprocessingwaterusedtospray,dip,rinse,orstorefoodbeforeprocessing,tobefol-lowedbyrinsinginpotablewaterorbyblanching,cooking,orcanning;sanitizerforhardsurfaces;broad-spectrumbacte-ricide,virucide,fungicide,andsporicide.REQUIREMENTSLeadNotmorethan1mg/kg.MercuryNotmorethan1mg/kg.pHBetween2.3and3.9.Note:ThepHischosendependingontheapplication;itcontrolstheconcentrationofmetastablechlorousacid,whichrapidlybreaksdownintochlorinedioxide,chlo-ride,andinsomeapplications,chlorate.Caution:Tominimizetheevolutionofhazardouschlo-rinedioxidegas,donotadjustthepHbelow2.3.SodiumChloriteBetween40and1200ppm,dependingontheapplication.TESTSLeadDetermineasdirectedunderLeadLimitTest,Appen-dixIIIB,usinga1.0-mLportionofsamplemixedwith5mLofwaterand11mLof2.7Nhydrochloricacid,and10goflead(Pb)ioninthecontrol.MercuryDetermineasdirectedunderMercuryLimitTest,AppendixIIIB,usingthefollowingastheSamplePrepara-tion:Transfer2.0mLofsampleintoa50-mLbeaker;add10mLofwater,1mLof1:5sulfuricacid,and1mLofa1:25potassiumpermanganatesolution;coverwithawatchglass;boilforafewseconds;andcool.pHDetermineasdirectedunderpHDetermination,Appen-dixIIB.SodiumChlorite(21CFR173.325;‘‘DeterminationofSo-diumChlorite:50ppmto1500ppm,’’AlcideCorporation)SampleForsolutionscontaining40to250ppm,usea100-gsample;forthosecontaining250to500ppm,usea50-gsample;forthosecontaining500to1100ppm,usea20-gsam-ple;forthosecontaining1100to1500ppm,usea15-gsample.ProcedureTransferthesampleintoatared250-mLErlen-meyerflask,andrecordtheweighttothenearest0.1mg.Addamagneticstirringbar.Addapproximately2gofpotassiumiodide,placetheflaskoveramagneticstirrer,andstiruntilthepotassiumiodidecrystalsdissolve(about1min).Add1mLof6Nhydrochloricacid,andstirfor30s.Whilecontinuouslystirring,titratetheliberatediodinewithstandardized0.025Nsodiumthiosulfate(Na2S2O3).Whenmostofthebrowniodinecolorhasfaded,add2mLofstarchindicatorsolution,andtitratetoaclearendpoint,allowingadequatemixingtimebetweenadditionsoftitrantneartheendpoint.Recordthevolumeoftitrant,V,inmilliliters.CalculationCalculatetheamountofSodiumChlorite,inpartspermillion,bytheequation16/AconiticAcid/Monographs食界论坛http://www.sinofood.com.cn/bbs.htm
FCCVppmofSodiumChlorite=(V×N×90.44×1000)/(W×4),inwhichVisthevolume,inmilliliters,oftitrant;Nisthenormalityofthesodiumthiosulfatetitrant;90.44isthemolec-ularweightofSodiumChlorite;1000isaconversionfactorfrommilligramspergramtopartspermillion;Wistheweight,ingrams,ofthesample;and4isthemilliequivalentsofsodiumthiosulfatepermilliequivalentofSodiumChlorite.AlternativeMethodsTheconcentrationofSodiumChloritealsocanbedeterminedusingionchromatogra-phybyfollowingU.S.EnvironmentalProtectionAgencyMethod300.11oramperometricallybyfollow-ingAmericanPublicHealthAssociationMethod4500-ClO2.2PackagingandStorageStoreinclosed,opaquecontainers.Avoidexposuretosunorultravioletlightbecausechlorinedioxidegaswillgenerateinthesolution.AconiticAcidEquiseticAcid;CitridicAcid;AchilleicAcid;1-Propene-1,2,3-tricarboxylicAcidHCCOOHHOOCCCH2COOHC6H6O6Formulawt174.11CAS:[499-12-7]FEMA:2010DESCRIPTIONAconiticAcidoccursintheleavesandtubersofAconitumnapellusL.(Fam.Ranunculaceae)andvariousspeciesofAchilleaandEquisetum,inbeetroot,andinsugarcane.Itmaybesynthesizedbythedehydrationofcitricacidbysulfuricormethanesulfonicacid.AconiticAcidfromtheabovesourceshasthe‘‘trans’’configuration.Ithasameltingpointof195°to200°withdecomposition.Itispracticallyodorlessandhasawinytaste.Itissolubleinwaterandinalcoholandisslightlysolubleinether.FunctionFlavoringsubstanceandadjuvant.1Hautman,DanielP.andMunch,DavidJ.‘‘Method300.1:Determina-tionofinorganicanionsindrinkingwaterbyionchromatography,Revi-sion1.0.’’U.S.EnvironmentalProtectionAgency,OfficeofGroundWaterandDrinkingWater.1997.Online.Available: AdipicAcidHexanedioicAcid;1,4-ButanedicarboxylicAcidHOOC(CH2)4COOHC6H10O4Formulawt146.14INS:355CAS:[124-04-9]DESCRIPTIONAdipicAcidoccursaswhitecrystalsoracrystallinepowder.Itisnothygroscopic.Itisfreelysolubleinalcohol,solubleinacetone,andslightlysolubleinwater.FunctionBuffer;neutralizingagent.REQUIREMENTSAssayNotlessthan99.6%andnotmorethan101.0%ofC6H10O4,calculatedontheanhydrousbasis.LeadNotmorethan2mg/kg.MeltingRangeBetween151.5°and154°.ResidueonIgnitionNotmorethan0.002%.WaterNotmorethan0.2%.TESTSAssayMixabout1.5gofsample,accuratelyweighed,with75mLofrecentlyboiledandcooledwatercontainedina250-mLglass-stopperedErlenmeyerflask,addphenolphtha-leinTS,andtitratewith0.5Nsodiumhydroxidetothefirstappearanceofafaintpinkendpointthatpersistsforatleast30s,shakingtheflaskastheendpointisapproached.Eachmilliliterof0.5Nsodiumhydroxideisequivalentto36.54mgofC6H10O4.LeadDetermineasdirectedinFlameAtomicAbsorptionSpectrophotometricMethodunderLeadLimitTest,AppendixIIIB,usinga5-gsample.MeltingRangeDetermineasdirectedunderMeltingRangeorTemperature,AppendixIIB.ResidueonIgnitionTransfer100.0gofsampleintoatared125-mLplatinumdishthathasbeenpreviouslycleanedbyfusingwith5gofpotassiumpyrosulfateorbisulfate,followedbyboilingin2Nsulfuricacidandrinsingwithwater.Meltthesamplecompletelyoveragasburner,thenignitethemeltwiththeburner.Afterignitionstarts,lowerorremovetheflametopreventthesamplefromboilingandtokeepitburningslowlyuntilitiscompletelycarbonized.Igniteat850°inamufflefurnacefor30minoruntilthecarboniscompletelyremoved,thencoolandweigh.WaterDetermineasdirectedunderWaterDetermination,AppendixIIB.PackagingandStorageStoreinwell-closedcontainers.AgarINS:406CAS:[9002-18-0]DESCRIPTIONAgariscommerciallyavailableaswhitetopaleyellowbundlesconsistingofthin,membranousagglutinatedstrips,orincut,flaked,granulated,orpowderedforms.AgarisagenericnamegiventoagroupofrelatedmoleculeswitharepeatingunitofagarobioseformedbasicallybyD-andL-galactoseunitsinterlinkedwith␣-1,3and-1,4linkages.Approximatelyev-erytenthD-galactopyranoseunitcontainsasulfateestergroup.Itisextractedfromthecellularwallsofagarophyteseaweed,consideringassuchtheredseaweedfromphylumRodophyta,whichbelongtotheGelidiceae,Gracilariaceae,andAhnphel-tiaceaefamilies.Itisinsolubleincoldwater,butitissolubleinboilingwater.FunctionStabilizer;emulsifier;thickener.REQUIREMENTSIdentificationA.Placeafewfragmentsofungroundsampleorasmallamountofthepowderonaslide,addafewdropsofwater,andexaminemicroscopically.Thesampleappearsgranularandsomewhatfilamentous.Afewfragmentsofthespiculesofspongesandafewfrustulesofdiatomsmaybepresent.B.Whilestirringcontinuously,boil1gofsamplewith65mLofwaterfor10min,andadjusttoaconcentrationof1.5%,byweight,withhotwater.Aclearliquidresultsthatcongealsbetween32°and39°toformafirm,resilientgelthatdoesnotliquefybelow85°.ArsenicNotmorethan3mg/kg.Ash(Acid-Insoluble)Notmorethan0.5%,calculatedonthedriedbasis.Ash(Total)Notmorethan6.5%,calculatedonthedriedbasis.GelatinPassestest.InsolubleMatterNotmorethan1.0%.LeadNotmorethan5mg/kg.LossonDryingNotmorethan20.0%.StarchPassestest.WaterAbsorptionPassestest.TESTSArsenicDetermineasdirectedunderArsenicLimitTest,AppendixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds.Ash(Acid-Insoluble)DetermineasdirectedunderAsh(Acid-Insoluble),AppendixIIC.Ash(Total)DetermineasdirectedunderAsh(Total),Ap-pendixIIC.GelatinDissolveabout1gofsamplein100mLofboilingwater,andallowthesolutiontocooltoabout50°.Add5mL18/DL-Alanine/Monographs食界论坛http://www.sinofood.com.cn/bbs.htm FCCVoftrinitrophenolTSto5mLofthesolution.Noturbidityformswithin10min.InsolubleMatterAddsufficientwaterto7.5gofsampletomake500g,boilfor15min,andreadjusttotheoriginalweight.Addhotwaterto100gofthemixturetomake200mL,heatalmosttoboiling,filterwhilehotthroughataredfilteringcrucible,rinsethecontainerwithseveralportionsofhotwater,andpasstherinsingsthroughthecrucible.Drythecrucibleanditscontentsat105°toconstantweight,cool,andweigh.Theweightoftheresiduedoesnotexceed15mg.LeadDetermineasdirectedunderLeadLimitTest,Appen-dixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds,and5goflead(Pb)ioninthecontrol.LossonDryingDetermineasdirectedunderLossonDry-ing,AppendixIIC,dryingasampleat105°for5h.Cutungroundsampleinto2-to5-mmsquarepiecesbeforedrying.StarchBoil100mgofsamplein100mLofwater,cool,andaddafewdropsofiodineTS.Nobluecolorappears.WaterAbsorptionPlace5gofsampleintoa100-mLgraduatedcylinder,filltovolumewithwater,mix,andallowtostandatabout25°for24h.Pourthecontentsofthecylinderthroughmoistenedglasswool,allowingthewatertodrainintoanother100-mLgraduatedcylinder.Notmorethan75mLofwaterisobtained.PackagingandStorageStoreinwell-closedcontainers.DL-AlanineDL-2-AminopropanoicAcidCH3CH(NH2)COOHC3H7NO2Formulawt89.09CAS:[302-72-7]View IRDESCRIPTIONDL-Alanineoccursasawhitecrystallinepowder.Itisfreelysolubleinwater,butsparinglysolubleinalcohol.ThepHofa1:20aqueoussolutionisbetween5.5and7.0.Itmeltswithdecompositionatabout198°.Itisopticallyinactive.FunctionNutrient.REQUIREMENTSIdentificationTheinfraredabsorptionspectrumofthesam-pleexhibitsrelativemaximaatthesamewavelengthsasthoseofatypicalspectrumasshowninthesectiononInfraredSpectra,usingthesametestconditionsasspecifiedtherein.AssayNotlessthan98.5%andnotmorethan101.5%ofC3H7NO2,calculatedonthedriedbasis.LeadNotmorethan5mg/kg.LossonDryingNotmorethan0.3%.ResidueonIgnitionNotmorethan0.2%.TESTSAssayDissolveabout200mgofsample,accuratelyweighed,in3mLofformicacidand50mLofglacialaceticacid,add2dropsofcrystalvioletTS,andtitratewith0.1Nperchloricacidtoablue-greenendpoint.Caution:Handleperchloricacidinanappropriatefumehood.Performablankdetermination(seeGeneralProvisions),andmakeanynecessarycorrection.Eachmilliliterof0.1Nper-chloricacidisequivalentto8.909mgofC3H7NO2.LeadDetermineasdirectedunderLeadLimitTest,Appen-dixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds,and5goflead(Pb)ioninthecontrol.LossonDryingDetermineasdirectedunderLossonDry-ing,AppendixIIC,dryingasampleat105°for3h.ResidueonIgnitionDetermineasdirectedunderResidueonIgnition,AppendixIIC,ignitinga1-gsample.PackagingandStorageStoreinwell-closed,light-resistantcontainers.L-AlanineL-2-AminopropanoicAcidCH3CCOOHHNH2C3H7NO2Formulawt89.09CAS:[56-41-7]View IRDESCRIPTIONL-Alanineoccursasawhitecrystallinepowder.Itisfreelysolubleinwater,sparinglysolubleinalcohol,andinsolubleinether.ThepHofa1:20aqueoussolutionisbetween5.5and7.0.FunctionNutrient.REQUIREMENTSIdentificationTheinfraredabsorptionspectrumofthesam-pleexhibitsrelativemaximaatthesamewavelengthsasthoseofatypicalspectrumasshowninthesectiononInfraredSpectra,usingthesametestconditionsasspecifiedtherein.AssayNotlessthan98.5%andnotmorethan101.5%ofC3H7NO2,calculatedonthedriedbasis.LeadNotmorethan5mg/kg.FCCVMonographs/AlginicAcid/19食界论坛http://www.sinofood.com.cn/bbs.htm LossonDryingNotmorethan0.3%.Optical(Specific)Rotation[␣]D20°:Between+15.5°,calculatedonthedriedbasis;or[␣]D25°+13.5°and:between+13.2°and+15.2°,calculatedonthedriedbasis.ResidueonIgnitionNotmorethan0.2%.TESTSAssayDissolveabout200mgofsample,accuratelyweighed,in3mLofformicacidand50mLofglacialaceticacid,add2dropsofcrystalvioletTS,andtitratewith0.1Nperchloricacidtoablue-greenendpoint.Caution:Handleperchloricacidinanappropriatefumehood.Performablankdetermination(seeGeneralProvisions),andmakeanynecessarycorrection.Eachmilliliterof0.1Nper-chloricacidisequivalentto8.909mgofC3H7NO2.LeadDetermineasdirectedunderLeadLimitTest,Appen-dixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds,and5goflead(Pb)ioninthecontrol.LossonDryingDetermineasdirectedunderLossonDry-ing,AppendixIIC,dryingasampleat105°for3h.Optical(Specific)RotationDetermineasdirectedunderOptical(Specific)Rotation,AppendixIIB,usingasolutioncontaining10gofapreviouslydriedsampleinsufficient6Nhydrochloricacidtomake100mL.ResidueonIgnitionDetermineasdirectedunderResidueonIgnition,AppendixIIC,ignitinga1-gsample.PackagingandStorageStoreinwell-closed,light-resistantcontainers.AlginicAcid(C6H8O6)nFormulawt,calculated176.13Formulawt,actual(avg.)200.00INS:400CAS:[9005-32-7]DESCRIPTIONAlginicAcidoccursasawhitetoyellow-white,fibrouspow-der.Itisahydrophiliccolloidalcarbohydrateextractedfromvariousspeciesofbrownseaweeds(phaeophyceae)withdilutealkali.Itmaybedescribedchemicallyasalinearglycurono-glycanconsistingmainlyof-1,4linkedD-mannuronicandL-guluronicacidunitsinthepyranoseringform.AlginicAcidisinsolubleinwater,readilysolubleinalkalinesolutions,andinsolubleinorganicsolvents.ThepHofa3:100suspensioninwaterisbetween2.0and3.4.FunctionStabilizer;thickener;emulsifier.REQUIREMENTSIdentificationA.Add1mLofcalciumchlorideTSto5mLofa1:150solutionofsamplein0.1Nsodiumhydroxide.Avoluminousgelatinousprecipitateforms.B.Add1mLof2Nsulfuricacidto5mLofthesolutionpreparedforIdentificationTestA.Aheavygelatinousprecipi-tateforms.C.Placeabout5mgofsampleintoatesttube,add5mLofwater,1mLofafreshlyprepared1:100naphtholresorcin-ol:ethanolsolution,and5mLofhydrochloricacid.Heatthemixturetoboiling,boilgentlyforabout3min,andthencooltoabout15°.Transferthecontentsofthetesttubetoa30-mLseparatorwiththeaidof5mLofwater,andextractwith15mLofisopropylether.Performablankdetermination(seeGeneralProvisions),andmakeanynecessarycorrection.Theisopropyletherextractfromthesampleexhibitsadeeperpurplehuethanthatfromtheblank.AssayAsampleyieldsnotlessthan20%andnotmorethan23%ofcarbondioxide(CO2),correspondingtobetween91.0%and104.5%of(C6H8O6)n(equivwt200.00),calculatedonthedriedbasis.ArsenicNotmorethan3mg/kg.LeadNotmorethan5mg/kg.LossonDryingNotmorethan15.0%.ResidueonIgnition(SulfatedAsh)Notmorethan8.0%,calculatedonthedriedbasis.TESTSAssayDetermineasdirectedunderAlginatesAssay,Appen-dixIIIC.Eachmilliliterof0.25Nsodiumhydroxideconsumedintheassayisequivalentto25mgof(C6H8O6)n(equivwt200.00).ArsenicDetermineasdirectedunderArsenicLimitTest,AppendixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds.LeadDetermineasdirectedunderLeadLimitTest,Appen-dixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds,and5gofleadion(Pb)inthecontrol.LossonDryingDetermineasdirectedunderLossonDry-ing,AppendixIIC,dryingasampleat105°for4h.ResidueonIgnition(SulfatedAsh)DetermineasdirectedinMethodIunderResidueonIgnition,AppendixIIC,ignitinga3-gsample.PackagingandStorageStoreinwell-closedcontainers.20/AlluraRed/Monographs食界论坛http://www.sinofood.com.cn/bbs.htm FCCVAlluraRed1AlluraRedAC;CI16035;Class:MonoazoOCH3HONaO3SNNH3CSO3NaC18H14N2O8S2Na2Formulawt496.43INS:129CAS:[25956-17-6]DESCRIPTIONAlluraRedoccursasared-brownpowderorgranule.Itisprincipallythedisodiumsaltof6-hydroxy-5-[(2-methoxy-5-methyl-4-sulfophenyl)azo]-2-naphthalenesulfonicacid.Itdis-solvesinwatertogiveasolutionredatneutralityandinacidanddarkredinbase.Itisinsolubleinethanol.FunctionColor.REQUIREMENTSIdentificationAnaqueoussolutioncontaining16.4mg/Lexhibitsabsorbanceintensities(A)andwavelengthmaximaasfollows:atpH7,A=0.87at500nm;atpH1,A=0.83at490nm(bothneutralandacidsolutionsexhibitashoulderatabout410nm);andatpH13,A=0.37at500nm,andA=0.41at450nm.AssayNotlessthan85.0%totalcoloringmatters.ArsenicNotmorethan3mg/kg.EtherExtractsNotmorethan0.2%.LeadNotmorethan10mg/kg.LossonDrying(VolatileMatter)at135°,Chlorides,andSulfates(assodiumsalts)Notmorethan15.0%incombi-nation.SubsidiaryColorsDisodium6-Hydroxy-5-[(2-methoxy-5-methyl-4-sulfophenyl)azo]-8-(2-methoxy-5-methyl-4-sulfophenoxy)-2-naphthalene-sulfonicAcidNotmorethan1.0%.HigherandLowerSulfonatedSubsidiaryColors(assodiumsalts)Notmorethan1.0%each.1TobeusedorsoldforusetocolorfoodthatismarketedintheUnitedStates,thiscoloradditivemustbefromabatchthathasbeencertifiedbytheU.S.FoodandDrugAdministration(FDA).IfitisnotfromanFDA-certifiedbatch,itisnotapermittedcoloradditiveforfooduseintheUnitedStates,evenifitiscompositionallyequivalent.ThenameFD&CRedNo.40canbeappliedonlytoFDA-certifiedbatchesofthiscoloradditive.AlluraRedisacommonnamegiventotheuncertifiedcolorant.SeethemonographentitledFD&CRedNo.40fordirectionsforproducinganFDA-certifiedbatch.UncombinedIntermediatesandProductsofSideReac-tions4-Amino-5-methoxy-o-toluenesulfonicAcidNotmorethan0.2%.Disodium6,6′-Oxybis(2-naphthalenesulfonicAcid)Notmorethan1.0%.Sodium6-Hydroxy-2-naphthalenesulfonicAcidNotmorethan0.3%.Water-InsolubleMatterNotmorethan0.2%.TESTSAssayDeterminethetotalcolorstrengthastheweightper-centofthesampletakenusingMethodsIandIIinTotalColorunderColors,AppendixIIIC.ExpresstheTotalColorastheaverageofthetworesults.MethodI(SamplePreparation)Transfer175to225mgofsample,accuratelyweighed,intoa1-Lvolumetricflask,dissolveinanddilutetovolumewithwater.Theabsorptivity(a)forAlluraRedis0.052mg/L/cmat502nm.MethodII(SamplePreparation)Transferapproximately0.2gofsample,accuratelyweighed,intothetitrationflask.Thestoichiometricfactor(Fs)forAlluraRedis8.06.ArsenicDetermineasdirectedunderArsenicLimitTest,AppendixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds.ChlorideDetermineasdirectedinSodiumChlorideunderColors,AppendixIIIC.EtherExtractsDetermineasdirectedinEtherExtractsunderColors,AppendixIIIC.LeadDetermineasdirectedunderLeadLimitTest,Appen-dixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds,and10goflead(Pb)ioninthecontrol.LossonDrying(VolatileMatter)at135°DetermineasdirectedinLossonDrying(VolatileMatter)underColors,AppendixIIIC.SubsidiaryColorsSolventSystemUseasolventsystemcomposedof20mLeachofacetonitrile,dioxane,ethylacetate,isoamylalcohol,andwaterand4mLofammoniumhydroxide.StandardSolutionTransferapproximately1gofpurifiedAlluraRed(freeofsubsidiarycolors),accuratelyweighed,intoa50-mLvolumetricflask.Add50mgeachoflowerandhighersulfonatedsubsidiarycolors,accuratelyweighed,dissolveinanddilutetovolumewithwater.Storeinthedark.SampleSolutionTransferapproximately2gofsample,accuratelyweighed,intoa100-mLvolumetricflask,dissolveinanddilutetovolumewithwater.ProcedureSpot3-LaliquotsofSampleSolutionandStandardSolutionsidebyside3cmfromthebottomofa20-×20-cmglassplatecoatedwitha0.25-mmlayerofSilicaGelG.Uptosevensamplesandstandardsmayberunsimultaneously.Whentheplatehasairdriedfor15min,developitinanunlinedtankequilibratedwiththeSolventSystemforatleast20min.Allowthesolventfronttoreachtowithin3cmfromthetopoftheplate.Allowtheplatetodryinafumehood,andbyvisualinspection,comparetheintensitiesofthelowerandhigherFCCVMonographs/AluminumAmmoniumSulfate/21食界论坛http://www.sinofood.com.cn/bbs.htm sulfonatedsubsidiarycolorswiththoseintheStandardSolu-tion.IfthesubsidiarycolorsintheSampleSolutionappearmoreconcentratedthanthoseintheStandardSolution,deter-minethequantityofeach,usingadensitometersettomonitortheabsorbancemaximumofeach.Calculatetheconcentra-tionsofthesubsidiarycolorsinpercent(P),ifpresentabove0.1%,bytheequationP=(A×p)/AS,inwhichAistheareaofthedensitometercurve,pisthepercentofsubsidiarycolorintheStandardSolution,andASistheareaofthedensitometercurveforthesubsidiarycolorintheStandardSolution.SulfateDetermineasdirectedinSodiumSulfateunderCol-ors,AppendixIIIC.UncombinedIntermediatesandProductsofSideReac-tionsDetermineasdirectedforMethodIIinUncombinedIntermediatesandProductsofSideReactionsunderColors,AppendixIIIC,injecting20LofthefollowingSamplePrep-aration:Transfer0.25gofsample,accuratelyweighed,intoa100-mLvolumetricflask.Dissolveinanddilutetovolumewith0.1Mdisodiumborate(Na2B4O7).Water-InsolubleMatterDetermineasdirectedinWater-InsolubleMatterunderColors,AppendixIIIC.PackagingandStorageStoreinwell-closedcontainers.AlmondOil,Bitter,FFPABitterAlmondOilFreefromPrussicAcidCAS:[8013-76-1]View IRDESCRIPTIONAlmondOil,Bitter,FFPA,occursasacolorlesstoslightlyyellowliquidwithastrongalmondaromaandaslightlyastringent,mildtaste.Itisavolatileoilobtainedfromthenutsofthebitteralmondtree,PrunusamygdalusBatschvar.amara(DeCandolle)Focke(Fam.Rosaceae),apricotkernel(PrunusarmeniacaL.),andotherfruitkernelscontainingamygdalin.Itispreparedbysteamdistillationofawater-macerated,powdered,andpressedcakethathasbeenspeciallytreatedandredistilledtoremovehydrocyanicacid.Itissolubleinmostfixedoilsandinpropyleneglycol,slightlysolubleinmineraloil,andinsolubleinglycerin.FunctionFlavoringagent.REQUIREMENTSIdentificationTheinfraredabsorptionspectrumofthesam-pleexhibitsrelativemaximaatthesamewavelengthsasthoseofatypicalspectrumasshowninthesectiononInfraredSpectra,usingthesametestconditionsasspecifiedtherein.AssayNotlessthan95.0%ofaldehydes,calculatedasbenz-aldehyde(C7H6O).AcidValueNotmorethan8.0.ChlorinatedCompoundsPassestest.HydrocyanicAcidPassestest(about0.015%).Optical(Specific)RotationOpticallyinactive,ornotmorethanϮ0.15°.RefractiveIndexBetween1.541and1.546at20°.SolubilityinAlcoholPassestest.SpecificGravityBetween1.040and1.050.TESTSAssayDetermineasdirectedunderAldehydes,AppendixVI,usingabout1mLofsample,accuratelyweighed,and53.05astheequivalencefactor(e)inthecalculation.AcidValueDetermineasdirectedunderAcidValue,Ap-pendixVI.ChlorinatedCompoundsDetermineasdirectedunderChlorinatedCompounds,AppendixVI.HydrocyanicAcidTransfer1mLofsampleintoatesttube.Add1mLofwater,5dropsofa1:10solutionofsodiumhydroxide,and5dropsofa1:10solutionofferroussulfate.Shakethoroughly,andacidifywith0.5Nhydrochloricacid.Noblueprecipitateorcolorappears.Optical(Specific)RotationDetermineasdirectedunderOptical(Specific)Rotation,AppendixIIB,usinga100-mmtube.RefractiveIndexDetermineasdirectedunderRefractiveIndex,AppendixIIB,usinganAbbe´orotherrefractometerofequalorgreateraccuracy.SolubilityinAlcoholDetermineasdirectedunderSolubilityinAlcohol,AppendixVI.Onemilliliterofsampledissolvestoformaclearsolutionin2mLof70%alcohol.SpecificGravityDeterminebyanyreliablemethod(seeGeneralProvisions).PackagingandStorageStoreinacoolplaceprotectedfromlightinfull,tightcontainersthataremadefromsteeloraluminumandthataresuitablylined.AluminumAmmoniumSulfateAmmoniumAlumAlNH4(SO4)2·12H2OFormulawt453.32INS:523CAS:[7784-25-0]DESCRIPTIONAluminumAmmoniumSulfateoccursaslarge,colorlesscrys-tals,whitegranules,orapowder.Onegramdissolvesin7mLofwaterat25°andinabout0.3mLofboilingwater.Its22/AluminumPotassiumSulfate/Monographs食界论坛http://www.sinofood.com.cn/bbs.htm FCCVsolutionsareacidtolitmus.Itisinsolubleinalcohol,andisfreely,butslowly,solubleinglycerin.FunctionBuffer;neutralizingagent.REQUIREMENTSIdentificationA1:20aqueoussolutiongivespositivetestsforAluminum,forAmmonium,andforSulfate,AppendixIIIA.AssayNotlessthan99.5%andnotmorethan100.5%ofAlNH4(SO4)2·12H2O.AlkaliesandAlkalineEarthsPassestest.FluorideNotmorethan0.003%.LeadNotmorethan3mg/kg.SeleniumNotmorethan0.003%.TESTSAssayDissolveabout1gofsample,accuratelyweighed,in50mLofwater,add50.0mLof0.05MdisodiumEDTAand20mLofpH4.5buffersolution(77.1gofammoniumacetateand57mLofglacialaceticacidin1000mLofsolution),andboilgentlyfor5min.Cool,andadd50mLofalcoholand2mLofdithizoneTS.Backtitratewith0.05Mzincsulfatetoabrightrose-pinkcolor.Performablankdetermination(seeGeneralProvisions),andmakeanyneces-sarycorrection.Themillilitersof0.05MdisodiumEDTAconsumedisequivalentto50minusthemillilitersof0.05Mzincsulfateused.Eachmilliliterof0.05MdisodiumEDTAconsumedisequivalentto22.67mgofAlNH4(SO4)2·12H2O.AlkaliesandAlkalineEarthsCompletelyprecipitatethealuminumfromaboilingsolutionof1gofsamplein100mLofwaterbyaddingenough6NammoniumhydroxidetorenderthesolutiondistinctlyalkalinetomethylredTS,andfilter.Evaporatethefiltratetodryness,andignite.Theweightoftheresiduedoesnotexceed5mg.FluorideDetermineasdirectedinMethodVunderFluorideLimitTest,AppendixIIIB.LeadDetermineasdirectedintheAPDCExtractionMethodunderLeadLimitTest,AppendixIIIB.SeleniumDetermineasdirectedinMethodIIunderSele-niumLimitTest,AppendixIIIB,usinga200-mgsample.PackagingandStorageStoreinwell-closedcontainers.AluminumPotassiumSulfatePotassiumAlumAlK(SO4)2·12H2OFormulawt474.38INS:522CAS:[7784-24-9]DESCRIPTIONAluminumPotassiumSulfateoccursaslarge,transparentcrys-talsorcrystallinefragments,orasawhitecrystallinepowder.Onegramdissolvesin7.5mLofwaterat25°andinabout0.3mLofboilingwater.Itssolutionsareacidtolitmus.Itisinsolubleinalcohol,butisfreelysolubleinglycerin.FunctionBuffer;neutralizingagent;firmingagent.REQUIREMENTSIdentificationA1:20aqueoussolutiongivespositivetestsforAluminum,forPotassium,andforSulfate,AppendixIIIA.AssayNotlessthan99.5%andnotmorethan100.5%ofAlK(SO4)2·12H2O.AmmoniumSaltsPassestest.FluorideNotmorethan0.003%.LeadNotmorethan3mg/kg.SeleniumNotmorethan0.003%.TESTSAssayDissolveabout1gofsample,accuratelyweighed,in50mLofwater,add50.0mLof0.05MdisodiumEDTAand20mLofpH4.5buffersolution(77.1gofammoniumacetateand57mLofglacialaceticacidin1000mLofaqueoussolution),andboilgentlyfor5min.Cool,andadd50mLofalcoholand2mLofdithizoneTS.Backtitratewith0.05Mzincsulfatetoabrightrose-pinkcolor.Performablankdetermination(seeGeneralProvisions),andmakeanyneces-sarycorrection.Themillilitersof0.05MdisodiumEDTAconsumedisequivalentto50minusthemillilitersof0.05Mzincsulfateused.Eachmilliliterof0.05MdisodiumEDTAisequivalentto23.72mgofAlK(SO4)2·12H2O.AmmoniumSaltsAdd1gofsampleto10mLof1Nsodiumhydroxideinasmallbeaker,andheatonasteambathfor1min.Theodorofammoniaisnotperceptible.FluorideDetermineasdirectedinMethodVunderFluorideLimitTest,AppendixIIIB.LeadDetermineasdirectedintheAPDCExtractionMethodunderLeadLimitTest,AppendixIIIB.SeleniumDetermineasdirectedinMethodIIunderSele-niumLimitTest,AppendixIIIB,usinga200-mgsample.PackagingandStorageStoreinwell-closedcontainers.AluminumSodiumSulfateSodaAlum;SodiumAlumAlNa(SO4)2Formulawt,anhydrous242.09AlNa(SO4)2·12H2OFormulawt,dodecahydrate458.29INS:521CAS:anhydrous[10102-71-3]CAS:dodecahydrate[7784-28-3]DESCRIPTIONAluminumSodiumSulfateoccursascolorlesscrystals,whitegranules,orapowder.ItisanhydrousormaycontainuptoFCCVMonographs/AluminumSulfate/23食界论坛http://www.sinofood.com.cn/bbs.htm 12moleculesofwaterofhydration.Theanhydrousformisslowlysolubleinwater.Thedodecahydrateisfreelysolubleinwater,anditefflorescesinair.Bothformsareinsolubleinalcohol.FunctionBuffer;neutralizingagent;firmingagent.REQUIREMENTSIdentificationAsamplerespondstotheflametestforSo-dium,AppendixIIIA,andgivespositivetestsforAluminumandforSulfate,AppendixIIIA.AssayAnhydrous:Notlessthan99.0%andnotmorethan104.0%ofAlNa(SO4)2afterdrying;Dodecahydrate:Notlessthan99.5%ofAlNa(SO4)2afterdrying.AmmoniumSaltsPassestest.FluorideNotmorethan0.003%.LeadNotmorethan3mg/kg.LossonDryingAnhydrous:Notmorethan10%;Dodecahy-drate:Notmorethan47.2%.NeutralizingValueAnhydrous:Between104and108.SeleniumNotmorethan0.003%.TESTSAssayAccuratelyweighabout500mgofsample,pre-viouslydriedasdirectedinthetestforLossonDrying(below),moistenwith1mLofglacialaceticacid,anddissolvein50mLofwater,warminggentlyonasteambathuntilsolutioniscomplete.Cool,neutralizewith6Nammoniumhydroxide,add50.0mLof0.05MdisodiumEDTAand20mLofpH4.5buffersolution(77.1gofammoniumacetateand57mLofglacialaceticacidin1000mLofaqueoussolution),andboilgentlyfor5min.Cool,andadd50mLofalcoholand2mLofdithizoneTS.Backtitratewith0.05Mzincsulfatetoabrightpinkcolor.Performablankdetermination(seeGeneralProvisions),andmakeanynecessarycorrection.Themillilitersof0.05MdisodiumEDTAconsumedisequivalentto50minusthemillilitersof0.05Mzincsulfateused.Eachmilliliterof0.05MdisodiumEDTAconsumedisequivalentto12.10mgofAlNa(SO4)2.AmmoniumSaltsHeat1gofsamplewith10mLof1Nsodiumhydroxideonasteambathfor1min.Theodorofammoniaisnotperceptible.FluorideDetermineasdirectedinMethodVundertheFluo-rideLimitTest,AppendixIIIB,usinga1.76-gsample.LeadDetermineasdirectedintheAPDCExtractionMethodunderLeadLimitTest,AppendixIIIB.LossonDryingAnhydrous:DetermineasdirectedunderLossonDrying,AppendixIIC,dryingasampleat200°for16h;Dodecahydrate:Determineasdirectedfortheanhydroussample,butdrythesamplefirstat50°to55°for1h,thenat200°for16h.NeutralizingValueTransfer500mgofanhydroussample,accuratelyweighed,intoa200-mLErlenmeyerflask,add30mLofwaterand4dropsofphenolphthaleinTS,andboiluntilthesampledissolves.Add13.0mLof0.5Nsodiumhydroxide,boilforafewseconds,andtitratewith0.5Nhydrochloricacidtothedisappearanceofthepinkcolor,add-ingtheaciddropwiseandagitatingvigorouslyaftereachaddition.Calculatetheneutralizingvalue,aspartsofNaHCO3equivalentto100partsofthesample,bytheformula8.4V,inwhichVisthevolume,inmilliliters,of0.5Nsodiumhydroxideconsumedbythesample.SeleniumDetermineasdirectedinMethodIIunderSele-niumLimitTest,AppendixIIIB,usinga200-mgsample.PackagingandStorageStoreintightcontainers.AluminumSulfateAl2(SO4)3Formulawt,anhydrous342.14Al2(SO4)3·18H2OFormulawt,octadecahydrate666.41INS:520CAS:anhydrous[10043-01-3]CAS:octadecahydrate[7784-31-8]DESCRIPTIONAluminumSulfateoccursasawhitepowder,asshiningplates,orascrystallinefragments.Itisanhydrousorcontains18moleculesofwaterofcrystallization.Becauseofefflores-cence,thehydratemayhaveacompositionapproximatingtheformulaAl2(SO4)3·14H2O.Onegramofthehydratedis-solvesinabout2mLofwater.Theanhydrousapproachesthesamesolubility,buttherateofsolutionissoslowthatitinitiallyappearstoberelativelyinsoluble.ThepHofa1:20aqueoussolutionis2.9orabove.FunctionFirmingagent.REQUIREMENTSIdentificationA1:10aqueoussolutiongivespositivetestsforAluminumandforSulfate,AppendixIIIA.AssayAnhydrous:Notlessthan99.5%ofAl2(SO4)3,calcu-latedontheignitedbasis;Octadecahydrate:Notlessthan99.5%andnotmorethan114.0%ofAl2(SO4)3·18H2O,corres-pondingtonotmorethanapproximately101.7%ofAl2(SO4)3·14H2O.AlkaliesandAlkalineEarthsPassestest(about0.4%).AmmoniumSaltsPassestest.FluorideNotmorethan0.003%.LeadNotmorethan3mg/kg.LossonIgnitionAnhydrous:Notmorethan5%.Note:ThisRequirementdoesnotapplytoAl2(SO4)3·18H2O.SeleniumNotmorethan0.003%.TESTSAssayAccuratelyweighanamountofsampleequivalenttoabout4gofAl2(SO4)3,transferintoa250-mLvolumetric24/AmbretteSeedOil/Monographs食界论坛http://www.sinofood.com.cn/bbs.htm FCCVflask,dissolveinanddilutetovolumewithwater,andmix.Pipet10mLofthissolutionintoa250-mLbeaker,add25.0mLof0.05MdisodiumEDTAand20mLofpH4.5buffersolution(77.1gofammoniumacetateand57mLofglacialaceticacidin1000mLofaqueoussolution),andboilgentlyfor5min.Cool,andadd50mLofalcoholand2mLofdithizoneTS.Backtitratewith0.05Mzincsulfatetoabrightpinkcolor.Performablankdetermination(seeGeneralProvi-sions),andmakeanynecessarycorrection.Themillilitersof0.05MdisodiumEDTAconsumedisequivalentto50minusthemillilitersof0.05Mzincsulfateused.Eachmilliliterof0.05MdisodiumEDTAconsumedisequivalentto8.554mgofAl2(SO4)3orto16.66mgofAl2(SO4)3·18H2O.AlkaliesandAlkalineEarthsAddafewdropsofmethylredTStoaboilingsolutionof2gofsamplein150mLofwater,andthenadd6Nammoniumhydroxideuntilthecolorofthesolutionjustchangestoadistinctyellow.Addhotwatertorestoretheoriginalvolume,andfilterwhilehot.Evaporate75mLofthefiltratetodryness,andignitetoconstantweight.Notmorethan4mgofresidueremains.AmmoniumSaltsHeat1gofsamplewith10mLof1Nsodiumhydroxideonasteambathfor1min.Theodorofammoniaisnotperceptible.FluorideDetermineasdirectedinMethodVundertheFluo-rideTest,AppendixIIIB,using1.67gofsample.LeadDetermineasdirectedintheAPDCExtractionMethodunderLeadLimitTest,AppendixIIIB.LossonIgnitionAnhydrous:Accuratelyweighabout2gofsample,andignite,preferablyinamufflefurnace,atabout500°for3h.Note:ThisTestdoesnotapplytoAl2(SO4)3·18H2O.SeleniumDetermineasdirectedinMethodIIunderSele-niumLimitTest,AppendixIIIB,usinga200-mgsample.PackagingandStorageStoreinwell-closedcontainers.AmbretteSeedOilAmbretteSeedLiquidCAS:[8015-62-1]View IRDESCRIPTIONAmbretteSeedOiloccursasaclearyellowtoamberliquidwiththestrong,muskyodorofambrettolide.ItisavolatileoilobtainedbysteamdistillationfromthepartiallydriedandcrushedseedsoftheplantAbelmoschusmoschatusMoench,syn.HibiscusabelmoschusL.(Fam.Malvaceae).Itisrefinedbysolventextractiontoremovefattyacidsorbyprecipitationofthefattyacidsalts.Itissolubleinmostfixedoilsandinmineraloil,oftenwithcloudiness,butrelativelyinsolubleinglycerinandinpropyleneglycol.FunctionFlavoringagent.REQUIREMENTSIdentificationTheinfraredabsorptionspectrumofthesam-pleexhibitsrelativemaximaatthesamewavelengthsasthoseofatypicalspectrumasshowninthesectiononInfraredSpectra,usingthesametestconditionsasspecifiedtherein.AcidValueNotmorethan3.0.Optical(Specific)RotationBetween–2.5°and+3°.RefractiveIndexBetween1.468and1.485at20°.SaponificationValueBetween140and200.SpecificGravityBetween0.898and0.920.TESTSAcidValueDetermineasdirectedunderAcidValue,Ap-pendixVI.Optical(Specific)RotationDetermineasdirectedunderOptical(Specific)Rotation,AppendixIIB,usinga100-mmtube.RefractiveIndexDetermineasdirectedunderRefractiveIndex,AppendixIIB,usinganAbbe´orotherrefractometerofequalorgreateraccuracy.SaponificationValueDetermineasdirectedinSaponifica-tionValueunderEsters,AppendixVI,usingabout1gofsample,accuratelyweighed.SpecificGravityDeterminebyanyreliablemethod(seeGeneralProvisions).PackagingandStorageStoreinacoolplaceprotectedfromlightinfull,tightcontainersthataremadefromsteeloraluminumandthataresuitablylined.AmmoniaSolutionAmmoniumHydroxide;StrongerAmmoniaWaterNH3Formulawt17.03INS:527CAS:[7664-41-7]DESCRIPTIONAmmoniaSolutionoccursasaclear,colorlessliquid.Uponexposuretoairitlosesammoniarapidly.Itsspecificgravityisabout0.90.Caution:AmmoniaSolutionisirritatingtotheoralmucosaandrespiratorytract.Performtestsinawell-ventilatedfumehood.FunctionpHcontrolagent;surfacefinishingagent;boilerwateradditive.REQUIREMENTSIdentificationHoldaglassrodwetwithhydrochloricacidnearthesurfaceofthesampleliquid.Dense,whitefumesevolve.FCCVMonographs/AmmoniatedGlycyrrhizin/25食界论坛http://www.sinofood.com.cn/bbs.htm AssayNotlessthan27.0%andnotmorethan30.0%,byweight,ofNH3.LeadNotmorethan0.5mg/kg.NonvolatileResidueNotmorethan0.02%.ReadilyOxidizableSubstancesPassestest.TESTSAssayAccuratelytarea125-mLglass-stopperedErlen-meyerflaskcontaining35.0mLof1Nsulfuricacid.Coolasample,containedinitsoriginalbottle,to10°orcooler.Partiallyfilla10-mLgraduatedpipetfromnearthebottomofthissample.(Donotusevacuumtodrawupthesample.)Wipeoffanyliquidadheringtotheoutsideofthepipet,anddiscardthefirstmilliliterofsample.Holdthepipetjustabovethesurfaceoftheacid,andtransfer2mLintotheflask,leavingatleast1mLinthepipet.Stoppertheflask,mix,andweighagaintoobtaintheweightofthesample.AddmethylredTS,andtitratetheexcessacidwith1Nsodiumhydroxide.Eachmilliliterof1Nsulfuricacidisequivalentto17.03mgofNH3.LeadDetermineasdirectedforMethodIintheAtomicAbsorptionSpectrophotometricGraphiteFurnaceMethodun-derLeadLimitTest,AppendixIIIB.NonvolatileResidueEvaporate11mL(10g)ofsampleinataredplatinumorporcelaindishtodryness,dryat105°for1h,cool,andweigh.ReadilyOxidizableSubstancesDilute4mLofsamplewith6mLofwater,andaddaslightexcessof2Nsulfuricacidand0.1mLof0.1Npotassiumpermanganate.Thepinkcolordoesnotcompletelydisappearwithin10min.PackagingandStorageStoreintightcontainersatatem-peraturenotexceeding25°.AmmoniatedGlycyrrhizinCAS:[1407-03-0]DESCRIPTIONAmmoniatedGlycyrrhizinoccursasabrownpowder.ItisprecipitatedbyacidfromthewaterextractofdriedandgroundrhizomesandrootsofGlycyrrhizaglabraorrelatedGlycyrr-hiza(licoriceroot)(Fam.Leguminosae)andneutralizedwithdiluteammonia.Suitablediluentsmaybeadded.FunctionFlavoringagent;flavorenhancer.REQUIREMENTSIdentificationAsamplegivespositivetestsforAmmonium,AppendixIIIA.AssayNotlessthan22.0%andnotmorethan32.0%ofmonoammoniumglycyrrhizinate(C42H65NO16),calculatedonthedriedbasis.Ash(Total)Notmorethan2.5%.LossonDryingNotmorethan6.0%.TESTSAssay(BasedonAOACmethod982.19.)Apparatus(SeeChromatography,AppendixIIA.)Useahigh-performanceliquidchromatographoperatedatroomtemperaturewitha10-mparticlesize,30-cm×4-mm(id),C18reverse-phasecolumn(BondapakC18column,WatersCorp.,34-TMapleStreet,Milford,MA01757,orequivalent).MaintaintheMobilePhaseatapressureandflowrate(typi-cally2.0mL/min)capableofgivingtherequiredelutiontime(seeSystemSuitabilityinHigh-PerformanceLiquidChroma-tography).Useanultravioletdetectorthatmonitorsabsorptionat254nm(0.2to0.1AUFSrange).MobilePhaseAdd380mLofacetonitrileand10mLofglacialaceticacidto610mLofglass-distilledwaterthathasbeenfilteredthrougha0.45-mfilter(Millipore,orequiva-lent).Mix,andde-gasthoroughly.StandardSolutionDissolveabout10mgofMonoammon-iumGlycyrrhizinateStandardforanalyticaluse(Sigma,orequivalent),accuratelyweighed,in20mLofa1:1(v/v)solutionofacetonitrile:water.Filterthesolutionthrougha0.45-mfilter(Millipore,orequivalent).Preparefreshdaily.Note:CorrecttheweightoftheMonoammoniumGly-cyrrhizinateStandardtakenforthepercentlossondry-ingshownonitslabel.AssaySolutionDissolveabout40gofsample,accuratelyweighed,in20mLofwater.Filterthesolutionthrougha0.45-mfilter(Millipore,orequivalent).SystemSuitabilityInjectduplicate10-LportionsoftheStandardSolutionintothechromatograph.Theretentiontimeofmonoammoniumglycyrrhizinateisapproximately6min.Adjusttheoperatingconditionsifnecessary.Themeanstan-darddeviationforreplicateinjectionsisnotmorethan2.0%.ProcedureSeparatelyinject,induplicate,10-LvolumesoftheStandardSolutionandtheAssaySolutionintothechromatograph,anddeterminethemeanpeakareaforeachsolution.Calculatethepercentmonoammoniumglycyrrhizi-nate,equivalenttoC42H65NO16,intheportionofsampletakenbytheformula100×(20CS/WU)×(AU/AS),inwhichCSistheconcentration,inmilligramspermilliliter,oftheStandardSolution;WUistheweight,inmilligrams,ofthesampletaken;andAUandASarethepeakareasoftheAssaySolutionandtheStandardSolution,respectively.Ash(Total)DetermineasdirectedunderAsh(Total),Ap-pendixIIC.LossonDryingDetermineasdirectedunderLossonDry-ing,AppendixIIC,dryinga1-gsampleat105°for1h.PackagingandStorageStoreinatightlyclosedcontainerinacool,dryplace.26/AmmoniumAlginate/Monographs食界论坛http://www.sinofood.com.cn/bbs.htm FCCVAmmoniumAlginateAlgin(C6H7O6NH4)nFormulawt,calculated193.16Formulawt,actual(avg.)217.00INS:403CAS:[9005-34-9]DESCRIPTIONAmmoniumAlginateoccursasawhitetoyellow,fibrousorgranularpowder.Itistheammoniumsaltofalginicacid(seethemonographforAlginicAcid).Itdissolvesinwatertoformaviscous,colloidalsolution.Itisinsolubleinalcoholandinhydroalcoholicsolutionsinwhichthealcoholcontentisgreaterthanabout30%byweight.Itisinsolubleinchloro-form,inether,andinacidshavingapHlowerthanabout3.FunctionStabilizer;thickener;emulsifier.REQUIREMENTSIdentificationA.Add1mLofcalciumchlorideTSto5mLofa1:100aqueoussolution.Avoluminous,gelatinousprecipitateforms.B.Add1mLof2.7Nsulfuricacidto10mLofa1:100aqueoussolution.Aheavy,gelatinousprecipitateforms.C.Placeabout5mgofsampleintoatesttube,add5mLofwater,1mLofafreshlyprepared1:100solutionnaphtholresorcinol:ethanol,and5mLofhydrochloricacid.Heatthemixturetoboiling,boilgentlyforabout3min,andthencooltoabout15°.Transferthecontentsofthetesttubetoa30-mLseparatorwiththeaidof5mLofwater,andextractwith15mLofisopropylether.Performablankdeter-mination(seeGeneralProvisions),andmakeanynecessarycorrection.Theisopropyletherextractfromthesampleexhib-itsadeeperpurplehuethanthatfromtheblank.D.Add5mLof1Nsodiumhydroxidetoabout1gofsamplecontainedinatesttube,andshakethemixturebriefly.Theodorofammoniaisevident.AssayAsampleyieldsnotlessthan18%andnotmorethan21%ofcarbondioxide(CO2),correspondingtobetween88.7%and103.6%ofAmmoniumAlginate(equivwt217.00),calculatedonthedriedbasis.ArsenicNotmorethan3mg/kg.LeadNotmorethan5mg/kg.LossonDryingNotmorethan15.0%.ResidueonIgnition(SulfatedAsh)Notmorethan7.0%,calculatedonthedriedbasis.TESTSAssayDetermineasdirectedunderAlginatesAssay,Appen-dixIIIC.Eachmilliliterof0.25Nsodiumhydroxideconsumedintheassayisequivalentto27.12mgofAmmoniumAlginate(equivwt217.00).ArsenicDetermineasdirectedunderArsenicLimitTest,AppendixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds.LeadDetermineasdirectedunderLeadLimitTest,Appen-dixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds,and5gofleadion(Pb)inthecontrol.LossonDryingDetermineasdirectedunderLossonDry-ing,AppendixIIC,dryingasampleat105°for4h.ResidueonIgnition(SulfatedAsh)DetermineasdirectedinMethodIunderResidueonIgnition,AppendixIIC,usinga3-gsample.PackagingandStorageStoreinwell-closedcontainers.AmmoniumBicarbonateNH4HCO3Formulawt79.06INS:503(ii)CAS:[1066-33-7]DESCRIPTIONAmmoniumBicarbonateoccursaswhitecrystalsorasacrys-tallinepowder.Itvolatilizesrapidlyat60°,dissociatingintoammonia,carbondioxide,andwater,butitisquitestableatroomtemperature.Onegramdissolvesinabout6mLofwater.Itisinsolubleinalcohol.FunctionAlkali;leaveningagent.REQUIREMENTSIdentificationAsamplegivespositivetestsforAmmoniumandforBicarbonate,AppendixIIIA.AssayNotlessthan99.0%andnotmorethan100.5%ofNH4HCO3.ChlorideNotmorethan0.003%.LeadNotmorethan3mg/kg.NonvolatileResidueNotmorethan0.05%(0.55%forprod-uctscontainingasuitableanticakingagent).SulfurCompounds(asSO4)Notmorethan0.007%.TESTSAssayDissolveabout3gofsample,accuratelyweighed,in40mLofwater.Add2dropsofmethylredTS,andwhileconstantlystirring,titratewith1Nhydrochloricacid,addingtheacidslowly,untilthesolutionbecomesfaintlypink.Heatthesolutiontoboiling,cool,andcontinuethetitrationuntilthefaintpinkcolornolongerfadesafterboiling.Eachmilliliterof1Nhydrochloricacidisequivalentto79.06mgofNH4HCO3.ChlorideDetermineasdirectedintheChlorideLimitTestunderChlorideandSulfateLimitTests,AppendixIIIB,usinga500-mgsample.Anyturbidityproducedbythesampledoesnotexceedthatproducedbyacontrolcontaining15gofchlorideion(Cl).LeadDetermineasdirectedintheAPDCExtractionMethodunderLeadLimitTest,AppendixIIIB.FCCVMonographs/AmmoniumChloride/27食界论坛http://www.sinofood.com.cn/bbs.htm NonvolatileResidueTransfer4gofsampleintoatareddish,add10mLofwater,andevaporatetodrynessonasteambath.Heatthedishat105°for1h,coolinadesiccator,andweigh.SulfurCompounds(asSO4)Dissolve4gofsamplein40mLofwater,addabout10mgofsodiumcarbonateand1mLof30%hydrogenperoxide,andevaporatethesolutiontodrynessonasteambath.TreattheresidueasdirectedintheSulfateLimitTestunderChlorideandSulfateLimitTests,AppendixIIIB.Anyturbidityproducedbythesampledoesnotexceedthatproducedbyacontrolcontaining280gofsulfateion(SO4).PackagingandStorageStoreinwell-closedcontainers.AmmoniumCarbonateINS:503(i)CAS:[10361-29-2]DESCRIPTIONAmmoniumCarbonateoccursasawhitepowderorashard,whiteortranslucentmasses.Itconsistsofammoniumbicarbon-ate(NH4HCO3)andammoniumcarbamate(NH2·COONH4)invaryingproportions.Onexposuretoairitbecomesopaqueandisfinallyconvertedintoporouslumpsorawhitepowderofammoniumbicarbonatebecauseofthelossofammoniaandcarbondioxide.Onegramdissolvesslowlyinabout4mLofwater.Itssolutionsarealkalinetolitmus.FunctionBuffer;leaveningagent;neutralizingagent.REQUIREMENTSIdentificationWhenheated,asamplevolatilizeswithoutcharring,andthevaporisalkalinetomoistenedlitmuspaper.A1:20aqueoussolutioneffervesceswhenanacidisadded.AssayNotlessthan30.0%andnotmorethan34.0%ofNH3.ChlorideNotmorethan0.003%.LeadNotmorethan3mg/kg.NonvolatileResidueNotmorethan0.05%.SulfurCompounds(asSO4)Notmorethan0.005%.TESTSAssayPlaceabout10mLofwaterinaweighingbottle,tarethebottleanditscontents,addabout2gofsample,andaccuratelyweigh.Transferthecontentsofthebottletoa250-mLflask,andwhilemixing,slowlyadd50.0mLof1Nsulfuricacid,allowingforthereleaseofcarbondioxide.Whensolutionhasbeeneffected,washdownthesidesoftheflaskwithafewmillilitersofwater,addafewdropsofmethylorangeTS,andtitratetheexcessacidwith1Nsodiumhydrox-ide.Eachmilliliterof1Nsulfuricacidisequivalentto17.03mgofNH3.ChlorideDetermineasdirectedintheChlorideLimitTestunderChlorideandSulfateLimitTests,AppendixIIIB,usingtheresidueofthefollowing:Dissolve500mgofsamplein10mLofhotwater,addabout5mgofsodiumcarbonate,andevaporatetodrynessonasteambath.Anyturbidityproduceddoesnotexceedthatshowninacontrolcontaining15gofchlorideion(Cl).LeadDetermineasdirectedintheAPDCExtractionMethodunderLeadLimitTest,AppendixIIIB.NonvolatileResidueTransfer4gofsampleintoatareddish,add10mLofwater,andevaporateonasteambath.Heatthedishat105°for1h,coolinadesiccator,andweigh.SulfurCompoundsDetermineasdirectedintheSulfateLimitTestunderChlorideandSulfateLimitTests,AppendixIIIB,usingtheresidueofthefollowing:Dissolve4gofsamplein40mLofwater,addabout10mgofsodiumcarbonateand1mLof30%hydrogenperoxide,andevaporatethesolutiontodrynessonasteambath.Anyturbidityproduceddoesnotexceedthatshowninacontrolcontaining200gofsulfate(SO4)ion.PackagingandStorageStoreintight,light-resistantcon-tainers,preferablyatatemperaturenotexceeding30°.AmmoniumChlorideNH4ClFormulawt53.49INS:510CAS:[12125-02-9]DESCRIPTIONAmmoniumChlorideoccursascolorlesscrystalsorasawhite,fineorcoarse,crystallinepowder.Itissomewhathygroscopic.Onegramdissolvesin2.6mLofwaterat25°,in1.4mLofboilingwater,inabout100mLofalcohol,andinabout8mLofglycerin.ThepHofa1:20solutionisbetween4.5and6.0.FunctionYeastfood;doughconditioner.REQUIREMENTSIdentificationA1:10aqueoussolutiongivespositivetestsforAmmoniumandforChloride,AppendixIIIA.AssayNotlessthan99.0%ofNH4Clafterdrying.LeadNotmorethan4mg/kg.LossonDryingNotmorethan0.5%.TESTSAssayDissolveabout200mgofsample,previouslydriedoversilicagelfor4handaccuratelyweighed,inabout40mLofwatercontainedinaglass-stopperedflask.Whileagitat-ingthemixture,add3mLofnitricacid,5mLofnitrobenzene,28/AmmoniumPhosphate,Dibasic/Monographs食界论坛http://www.sinofood.com.cn/bbs.htm FCCVand50.0mLof0.1Nsilvernitrate;shakevigorously;add2mLofferricammoniumsulfateTS;andtitratetheexcesssilvernitratewith0.1Nammoniumthiocyanate.Eachmilliliterof0.1Nsilvernitrateisequivalentto5.349mgofNH4Cl.LeadDetermineasdirectedunderLeadLimitTest,Appen-dixIIIB,using4goflead(Pb)ioninthecontrolLossonDryingDetermineasdirectedunderLossonDry-ing,AppendixIIC,dryingasampleoversilicagelfor4h.PackagingandStorageStoreintightcontainers.AmmoniumPhosphate,DibasicDiammoniumHydrogenPhosphate;DiammoniumPhosphate(NH4)2HPO4Formulawt132.06INS:342(ii)CAS:[7783-28-0]DESCRIPTIONAmmoniumPhosphate,Dibasic,occursaswhitecrystals,acrystallinepowder,orgranules.Itisfreelysolubleinwater.ThepHofa1:100aqueoussolutionisbetween7.6and8.2.FunctionBuffer;doughconditioner;leaveningagent;yeastfood.REQUIREMENTSIdentificationA1:20aqueoussolutiongivespositivetestsforAmmoniumandforPhosphate,AppendixIIIA.AssayNotlessthan96.0%andnotmorethan102.0%of(NH4)2HPO4.ArsenicNotmorethan3mg/kg.FluorideNotmorethan10mg/kg.LeadNotmorethan4mg/kg.TESTSAssayDissolveabout600mgofsample,accuratelyweighed,in40mLofwater,andtitratetoapHof4.6with0.1Nsulfuricacid.Eachmilliliterof0.1Nsulfuricacidisequivalentto13.21mgof(NH4)2HPO4.ArsenicDetermineasdirectedunderArsenicLimitTest,AppendixIIIB,usingasolutionof1gofsamplein35mLofwater.FluorideDetermineasdirectedinMethodIVunderFluo-rideLimitTest,AppendixIIIB,usinga2-gsample,BufferSolutionA,and0.1mLofFluorideStandardSolution.LeadDetermineasdirectedintheAPDCExtractionMethodunderLeadLimitTest,AppendixIIIB.PackagingandStorageStoreintightlyclosedcontainers.AmmoniumPhosphate,MonobasicAmmoniumDihydrogenPhosphate;MonoammoniumPhosphateNH4H2PO4Formulawt115.03INS:342(i)CAS:[7722-76-1]DESCRIPTIONAmmoniumPhosphate,Monobasic,occursaswhitecrystals,acrystallinepowder,orgranules.Itisfreelysolubleinwater.ThepHofa1:100aqueoussolutionisbetween4.3and5.0.FunctionBuffer;doughconditioner;leaveningagent;yeastfood.REQUIREMENTSIdentificationA1:20aqueoussolutiongivespositivetestsforAmmoniumandforPhosphate,AppendixIIIA.AssayNotlessthan96.0%andnotmorethan102.0%ofNH4H2PO4.ArsenicNotmorethan3mg/kg.FluorideNotmorethan10mg/kg.LeadNotmorethan4mg/kg.TESTSAssayDissolveabout500mgofsample,accuratelyweighed,in50mLofwater,andtitratetoapHof8.0with0.1Nsodiumhydroxide.Eachmilliliterof0.1Nsodiumhydroxideisequivalentto11.50mgofNH4H2PO4.ArsenicDetermineasdirectedunderArsenicLimitTest,Ap-pendixIIIB,usingasolutionof1gofsamplein35mLofwater.FluorideDetermineasdirectedinMethodIVundertheFluo-rideLimitTest,AppendixIIIB,usinga2-gsample,BufferSolu-tionB,and0.1mLofFluorideStandardSolution.LeadDetermineasdirectedintheAPDCExtractionMethodunderLeadLimitTest,AppendixIIIB.PackagingandStorageStoreintightlyclosedcontainers.AmmoniumSaccharin1,2-Benzisothiazolin-3-one1,1-DioxideAmmoniumSaltNNH4SO2C7H8N2O3SFormulawt200.21DESCRIPTIONAmmoniumSaccharinoccursaswhitecrystalsoraswhite,FCCVMonographs/AmmoniumSaccharin/29食界论坛http://www.sinofood.com.cn/bbs.htm crystallinepowder.Itisfreelysolubleinwater.ThepHofa1:3aqueoussolutionisbetween5and6.FunctionNonnutritivesweetener.REQUIREMENTSIdentificationA.Dissolveabout100mgofsamplein5mLofa1:20solutionofsodiumhydroxide,evaporatetodryness,andgentlyfusetheresidueoverasmallflameuntilammonianolongerevolves.Aftertheresiduehascooled,dissolveitin20mLofwater,neutralizethesolutionwith2.7Nhydrochloricacid,andfilter.Add1dropofferricchlorideTStothefiltrate.Avioletcolorappears.B.Mix20mgofsamplewith40mgofresorcinol,cau-tiouslyadd10dropsofsulfuricacid,andheatthemixtureinaliquidbathat200°for3min.Aftercooling,add10mLofwaterandanexcessof1Nsodiumhydroxide.Afluorescentgreenliquidresults.C.A1:10aqueoussolutiongivespositivetestsforAmmo-nium,AppendixIIIA.D.Add1mLofhydrochloricacidto10mLofa1:10aqueoussolution.Acrystallineprecipitateofsaccharinforms.Washtheprecipitatewellwithcoldwateranddryat105°for2h.Thesaccharinthusobtainedmeltsbetween226°and230°(seeMeltingRangeorTemperature,AppendixIIB).AssayNotlessthan98.0%andnotmorethan101.0%ofC7H8N2O3S,calculatedontheanhydrousbasis.BenzoateandSalicylatePassestest.LeadNotmorethan2mg/kg.ReadilyCarbonizableSubstancesPassestest.SeleniumNotmorethan0.003%.ToluenesulfonamidesNotmorethan0.0025%.WaterNotmorethan0.3%.TESTSAssayWiththeaidof10mLofwater,quantitativelytransferabout500mgofsample,accuratelyweighed,intoaseparatorAdd2mLof2.7Nhydrochloricacid,andextracttheprecipi-tatedsaccharin,firstwith30mL,thenwithfive20-mLpor-tionsofasolventcomprising9:1(v/v)chloroform:alcohol.Filtereachextractthroughasmallfilterpapermoistenedwiththesolventmixture,andevaporatethecombinedfiltratestodrynessonasteambathwiththeaidofacurrentofair.Dissolvetheresiduein75mLofhotwater,cool,addphenol-phthaleinTS,andtitratewith0.1Nsodiumhydroxide.Per-formablankdetermination(seeGeneralProvisions),andmakeanynecessarycorrection.Eachmilliliterof0.1Nsodiumhydroxideisequivalentto20.02mgofC7H8N2O3S.BenzoateandSalicylateAdd3dropsofferricchlorideTSto10mLofa1:20aqueoussolutionpreviouslyacidifiedwith5dropsofglacialaceticacid.Noprecipitateorvioletcolorappears.LeadDetermineasdirectedintheFlameAtomicAbsorptionSpectrophotometricMethodunderLeadLimitTest,AppendixIIIB,usinga10-gsample.ReadilyCarbonizableSubstancesDetermineasdirectedunderReadilyCarbonizableSubstances,AppendixIIB,using200mgofsampledissolvedin5mLof95%sulfuricacidandkeptat48°to50°for10min.ThecolorisnodarkerthanthatofMatchingFluidA.SeleniumDetermineasdirectedinMethodIundertheSele-niumLimitTest,AppendixIIIB,usinga200-mgsample.ToluenesulfonamidesMethyleneChlorideUseasuitablegrade(suchasthatobtainablefromBurdick&JacksonLaboratories,Inc.),equiv-alenttotheproductobtainedbydistillationinanall-glassapparatus.InternalStandardStockSolutionTransfer100.0mgof95%n-tricosane(obtainablefromChemicalSamplesCo.)intoa10-mLvolumetricflask,dissolveinanddilutetovolumewithn-heptane,andmix.StockStandardPreparationTransfer20.0mgeachofreagent-gradeo-toluenesulfonamideandp-toluenesulfon-amideintoa10-mLvolumetricflask,dissolveinanddilutetovolumewithmethylenechloride,andmix.DilutedStandardPreparationsPipet0.1,0.25,1.0,2.5,and5.0mL,respectively,oftheStockStandardPreparationintofive10-mLvolumetricflasks.Pipet0.25mLoftheInter-nalStandardStockSolutionintoeachflask,diluteeachtovolumewithmethylenechloride,andmix.Thesesolutionscontain,respectively,20,50,200,500,and1000g/mLofeachtoluenesulfonamide,plus250gofn-tricosane.TestPreparation(SeeChromatography,AppendixIIA.)Dissolve2.00gofsamplein8.0mLof5%sodiumbicarbonatesolution,andmixthesolutionthoroughlywith10.0gofchromatographicsiliceousearth(Celite545,Johns-Manville,orequivalent).Transferthemixtureintoa250-×25-mmchromatographictubehavingafritted-glassdiskandaTeflonstopcockatthebottomandareservoiratthetop.Packthecontentsofthetubebytappingthecolumnonapaddedsurface,andthenbytampingfirmlyfromthetop.Place100mLofmethylenechlorideinthereservoir,andadjustthestopcocksothat50mLofeluateiscollectedin20to30min.Add25LofInternalStandardStockSolutiontotheeluate,mix,andthenconcentratethesolutiontoavolumeof1.0mLinasuitableconcentratortubefittedwithamodifiedSnydercolumn,usingaKontestubeheatermaintainedat90°.ProcedureInject2.5LoftheTestPreparationintoasuitablegaschromatographequippedwithaflame-ionizationdetectoranda3-m×2-mm(id)glasscolumn,orequivalent,packedwith3%phenylmethylsilicone(OV-17,AppliedScienceLaboratories,Inc.,orequivalent)on100-to120-mesh,silanized,calcined,diatomaceoussilica(Gas-ChromQ,AppliedScience,orequivalent).Caution:Theglasscolumnshouldextendintotheinjec-torforon-columninjectionandintothedetectorbasetoavoidcontactwithmetal.Maintainthecolumnat108°.Settheinjectionporttemperatureto225°andthedetectorto250°.Useheliumasthecarriergas,withaflowrateof30mL/min.Settheinstrumentattenuationsettingsothat2.5LoftheDilutedStandardPreparationcontaining200g/mLofeachtoluenesulfonamidegivesaresponseof40%to80%offull-scaledeflection.Recordthe30/AmmoniumSulfate/Monographs食界论坛http://www.sinofood.com.cn/bbs.htm FCCVchromatogram,notethepeaksforo-toluenesulfonamide,p-toluenesulfonamide,andthen-tricosaneinternalstandard,andcalculatetheareasforeachpeakbysuitablemeans.Theretentiontimesforo-toluenesulfonamide,p-toluenesulfon-amide,andn-tricosaneareabout5,6,and15min,respectively.Inasimilarmanner,obtainthechromatogramsfor2.5-LportionsofeachofthefiveDilutedStandardPreparations,andforeachsolution,determinetheareasoftheo-toluenesul-fonamide,p-toluenesulfonamide,andn-tricosanepeaks.Fromthevaluesthusobtained,preparestandardcurvesbyplottingconcentrationofeachtoluenesulfonamide,inmicrogramspermilliliter,versustheratiooftherespectivetoluenesulfonamidepeakareatothatofn-tricosane.Fromthestandardcurve,determinetheconcentration,inmicrogramspermilliliter,ofeachtoluenesulfonamideintheTestPreparation.Divideeachvalueby2toconverttheresulttomilligramsperkilogramofthetoluenesulfonamideinthe2-gsampletakenforanalysis.Note:Ifthetoluenesulfonamidecontentofthesampleisgreaterthanabout500mg/kg,theimpuritymaycrystallizeoutofthemethylenechlorideconcentrate(seeTestPreparation).Althoughthislevelofimpurityexceedsthatpermittedbythespecification,theanalysismaybecompletedbydilutingtheconcentratewithmethylenechloridecontaining250gofn-tricosanepermilliliter,andbyapplyingappropriatedilutionfactorsinthecalculation.Caremustbetakentoredissolvecompletelyanycrystallinetoluenesulfonamidetogiveahomogeneoussolution.WaterDetermineasdirectedunderWaterDetermination,AppendixIIB.PackagingandStorageStoreinwell-closedcontainers.AmmoniumSulfate(NH4)2SO4Formulawt132.14INS:517CAS:[7783-20-2]DESCRIPTIONAmmoniumSulfateoccursascolorlessorwhitecrystalsorgranulesthatdecomposeattemperaturesabove280°.Onegramissolubleinabout1.5mLofwater.Itisinsolubleinalcohol.ThepHofa0.1Msolutionisbetween4.5and6.0.FunctionDoughconditioner;yeastnutrient.REQUIREMENTSIdentificationAsamplegivespositivetestsforAmmoniumandforSulfate,AppendixIIIA.AssayNotlessthan99.0%andnotmorethan100.5%of(NH4)2SO4.LeadNotmorethan3mg/kg.ResidueonIgnitionNotmorethan0.25%.SeleniumNotmorethan0.003%.TESTSAssayTransferabout2gofsample,accuratelyweighed,intoa250-mLflask,anddissolveitin100mLofwater.Add40mLofamixtureofequalvolumesofformaldehydeandwater,previouslyneutralizedtophenolphthaleinTSwith1Nsodiumhydroxide.Mix,allowtostandfor30min,andtitratethemixturewith1Nsodiumhydroxidetoapinkendpointthatpersistsfor5min.Eachmilliliterof1Nsodiumhydroxideisequivalentto66.06mgof(NH4)2SO4.LeadDetermineasdirectedintheAPDCExtractionMethodunderLeadLimitTest,AppendixIIIB.ResidueonIgnitionDetermineasdirectedunderResidueonIgnition,AppendixIIC,ignitinga1-gsample.SeleniumDetermineasdirectedinMethodIIunderSele-niumLimitTest,AppendixIIIB,using200mgofsample.PackagingandStorageStoreinwell-closedcontainers.AmyrisOil,WestIndianTypeSandalwoodOil,WestIndianTypeView IRDESCRIPTIONAmyrisOil,WestIndianType,occursasaclear,paleyellow,viscousliquidhavingadistinctodorsuggestiveofsandal-wood.ItisthevolatileoilobtainedbysteamdistillationfromthewoodofAmyrisbalsamiferaL.(Fam.Rutaceae).Itissolubleinmostfixedoilsandusuallyinmineraloil.Itissolubleinanequalvolumeofpropyleneglycol,thesolutionoftenbecomingopalescentonfurtherdilution.Itispracticallyinsolubleinglycerin.FunctionFlavoringagent.REQUIREMENTSIdentificationTheinfraredabsorptionspectrumofthesam-pleexhibitsrelativemaximaatthesamewavelengthsasthoseshownintherespectivespectruminthesectiononInfraredSpectra,usingthesametestconditionsasspecifiedtherein.AcidValueNotmorethan3.0.AngularRotationBetween+10°and+53°.EsterValueNotmorethan7.EsterValueafterAcetylationBetween115and165.RefractiveIndexBetween1.503and1.512at20°.SolubilityinAlcoholPassestest.SpecificGravityBetween0.943and0.976.FCCVMonographs/AngelicaSeedOil/31食界论坛http://www.sinofood.com.cn/bbs.htm TESTSAcidValueDetermineasdirectedunderAcidValue,Ap-pendixVI.AngularRotationDetermineasdirectedunderOptical(Specific)Rotation,AppendixIIB,usinga100-mmtube.EsterValueDetermineasdirectedinEsterValueunderEsters,AppendixVI,usingabout5gofsample,accuratelyweighed.EsterValueafterAcetylationDetermineasdirectedunderTotalAlcohols,AppendixVI,usingabout2gofthedriedacetylatedoil,accuratelyweighed.Refluxforaperiodof2h.CalculatetheEsterValueafterAcetylationbytheformulaA×28.05/B,inwhichAisthenumberofmillilitersof0.5Nalcoholicpotassiumhydroxideconsumedinthesaponification,andBistheweight,ingrams,oftheacetylatedoilusedinthetest.RefractiveIndexDetermineasdirectedunderRefractiveIndex,AppendixIIB,usinganAbbe´orotherrefractometerofequalorgreateraccuracy.SolubilityinAlcoholDetermineasdirectedunderSolubilityinAlcohol,AppendixVI.Onemilliliterofsampledissolvesin3mLof80%alcohol,oftenwithopalescence.SpecificGravityDeterminebyanyreliablemethod(seeGeneralProvisions).PackagingandStorageStoreinacoolplaceprotectedfromlightinfull,tightcontainersthataremadeofaluminumorglassorthatarelinedwithtin.AngelicaRootOilCAS:[8015-64-3]View IRDESCRIPTIONAngelicaRootOiloccursasapaleyellowtodeepamberliquidwithawarm,pungentodorandbittersweettaste.ItisobtainedbysteamdistillationofthedriedslenderrootletsofAngelicaarchangelicaL.(Fam.Umbelliferae).Itissolubleinmostfixedoils,slightlysolubleinmineraloil,butrelativelyinsolubleinglycerinandinpropyleneglycol.FunctionFlavoringagent.REQUIREMENTSIdentificationTheinfraredabsorptionspectrumofthesam-pleexhibitsrelativemaximaatthesamewavelengthsasthoseofatypicalspectrumasshowninthesectiononInfraredSpectra,usingthesametestconditionsasspecifiedtherein.AcidValueNotmorethan7.0.AngularRotationBetween0°and+46°.EsterValueBetween10and65.RefractiveIndexBetween1.473and1.487at20°.SolubilityinAlcoholPassestest.SpecificGravityBetween0.850and0.880.TESTSAcidValueDetermineasdirectedunderAcidValue,Ap-pendixVI.AngularRotationDetermineasdirectedunderOptical(Specific)Rotation,AppendixIIB,usinga100-mmtube.EsterValueDetermineasdirectedunderEsterValue,Ap-pendixVI,usingabout5gofsample,accuratelyweighed.RefractiveIndexDetermineasdirectedunderRefractiveIndex,AppendixIIB,usinganAbbe´orotherrefractometerofequalorgreateraccuracy.SolubilityinAlcoholDetermineasdirectedunderSolubilityinAlcohol,AppendixVI.Onemilliliterofsampledissolvesin1mLof90%alcohol,oftenwithturbidity,andremainsinsolutiononfurtheradditionofalcoholtoatotalof10mL.SpecificGravityDeterminebyanyreliablemethod(seeGeneralProvisions).PackagingandStorageStoreinacoolplaceprotectedfromlightinfull,tightcontainersthataremadefromsteeloraluminumandthataresuitablylined.Theoilincreasesinspecificgravityandviscosityduringstorage.AngelicaSeedOilView IRDESCRIPTIONAngelicaSeedOiloccursasalightyellowliquidhavingasweeterandmoredelicatearomathantherootoil.ItisobtainedbysteamdistillationofthefreshseedsofAngelicaarchan-gelicaL.(Fam.Umbelliferae).Itissolubleinmostfixedoils,slightlysolubleinmineraloil,butrelativelyinsolubleinglycerinandinpropyleneglycol.FunctionFlavoringagent.REQUIREMENTSIdentificationTheinfraredabsorptionspectrumofthesam-pleexhibitsrelativemaximaatthesamewavelengthsasthoseshownintherespectivespectruminthesectiononInfraredSpectra,usingthesametestconditionsasspecifiedtherein.AcidValueNotmorethan3.0.AngularRotationBetween+4°and+16°.EsterValueBetween14.0and32.0.RefractiveIndexBetween1.480and1.488at20°.SolubilityinAlcoholPassestest.SpecificGravityBetween0.853and0.876.32/AniseOil/Monographs食界论坛http://www.sinofood.com.cn/bbs.htm FCCVTESTSAcidValueDetermineasdirectedunderAcidValue,Ap-pendixVI.AngularRotationDetermineasdirectedunderOptical(Specific)Rotation,AppendixIIB,usinga100-mmtube.EsterValueDetermineasdirectedunderEsterDetermina-tion,AppendixVI,usingabout5gofsample,accuratelyweighed.RefractiveIndexDetermineasdirectedunderRefractiveIndex,AppendixIIB,usinganAbbe´orotherrefractometerofequalorgreateraccuracy.SolubilityinAlcoholDetermineasdirectedunderSolubilityinAlcohol,AppendixVI.Onemilliliterofsampledissolvesin4mLof90%alcohol,oftenwithconsiderableturbidity,anditremainsinsolutiononfurtheradditionofalcoholtoatotalof10mL.SpecificGravityDeterminebyanyreliablemethod(seeGeneralProvisions).PackagingandStorageStoreinacoolplaceprotectedfromlightinfull,tightcontainersthataremadefromsteeloraluminumandthataresuitablylined.AniseOilCAS:[8007-70-3]View IRDESCRIPTIONAniseOiloccursasacolorlesstopaleyellow,stronglyrefrac-tiveliquidwiththecharacteristicodorandtasteofanise.ItisobtainedbysteamdistillationofthedriedripefruitofPimpinellaanisumL.(Fam.Umbelliferae)orIlliciumverumHookerfilius(Fam.Magnoliaceae).Note:Ifsolidmaterialhasseparated,carefullywarmthesampleuntilitiscompletelyliquefied,andmixbeforeusingit.FunctionFlavoringagent.REQUIREMENTSIdentificationTheinfraredabsorptionspectrumofthesam-pleexhibitsrelativemaximaatthesamewavelengthsasthoseofatypicalspectrumasshowninthesectiononInfraredSpectra,usingthesametestconditionsasspecifiedtherein.AngularRotationBetween+1°and–1°.PhenolsPassestest.RefractiveIndexBetween1.553and1.560at20°.SolidificationPointNotlowerthan15°.SolubilityinAlcoholPassestest.SpecificGravityBetween0.978and0.988.TESTSAngularRotationDetermineasdirectedunderOptical(Specific)Rotation,AppendixIIB,usinga100-mmtube.PhenolsPreparea1:3solutionofrecentlydistilledsamplein90%alcohol.Itisneutraltomoistenedlitmuspaper,andadding1dropofferricchlorideTSto5mLofthesolutionproducesnoblueorbrowncolor.RefractiveIndexDetermineasdirectedunderRefractiveIndex,AppendixIIB,usinganAbbe´orotherrefractometerofequalorgreateraccuracy.SolidificationPointDetermineasdirectedunderSolidifica-tionPoint,AppendixIIB.SolubilityinAlcoholDetermineasdirectedunderSolubilityinAlcohol,AppendixVI,using3mLof90%alcohol.SpecificGravityDeterminebyanyreliablemethod(seeGeneralProvisions).PackagingandStorageStoreinacoolplaceprotectedfromlightinfull,tightcontainersthataremadefromsteeloraluminumandthataresuitablylined.AnnattoExtractsINS:160bCAS:[1393-63-1]DESCRIPTIONAnnattoExtractsoccurasdarkredsolutions,emulsions,orsuspensionsinwateroroilorasdarkredpowders.Theextractispreparedfromannattoseed,BixaorellanaL.(Fam.Bixa-ceae),usingafood-gradeextractionsolvent.Bixinistheprincipalpigmentofoil-solubleAnnattoExtracts.Norbixinistheprincipalpigmentofalkalinewater-solubleAnnattoExtracts.Commercialpreparationsareusuallymixturesofbixin,norbixin,andothercarotenoids.FunctionColor.REQUIREMENTSIdentificationA.Oil-andWater-SolubleAnnattoExtractsOil-solubleAnnattoExtractsdilutedwithacetoneexhibitabsorbancemax-imaat439,470,and501nm.Water-solubleAnnattoExtractsdilutedwithwaterexhibitabsorbancemaximaat451to455nmand480to484nm.B.Carr-PriceReaction(SeeChromatography,Appen-dixIIA.)Prepareasmallchromatographycolumnbyfillinga200-×7-mmglasstube,stopperedwithglasswool,withalumina(80-to200-mesh)slurriedintoluenesothatthesettledaluminafillsabout2⁄3ofthetube.Usingarubberoutlettubeandclamp,adjusttheflowratetoabout30drops/min.Oil-SolubleAnnattoExtractsAddtothetopofthealu-minacolumn3mLofasolutioncontainingsufficientsample,FCCVMonographs/-Apo-8′-Carotenal/33食界论坛http://www.sinofood.com.cn/bbs.htm intoluene,toimpartacolorequivalenttoasolutionof0.1%potassiumdichromate.Elutewithtolueneuntilapaleyellowfractioniswashedfromthecolumn.Washthecolumnwiththree10-mLvolumesofdryacetone,add5mLofCarr-PriceReagent(seeSolutionsandIndicators),andallowittorunontothetopofthecolumn.Theorange-redzone(bixin)atthetopofthecolumnimmediatelyturnsblue-green.Water-SolubleAnnattoExtractsTransfer2mLor2gofsampleintoa50-mLseparatoryfunnel,andaddsufficient2NsulfuricacidtomakethesolutionacidictopHtestpaper(pH1to2).Dissolvetheredprecipitateofnorbixinbymixingthesolutionwith50mLoftoluene.Discardthewaterlayer,andwashthetoluenephasewithwateruntilitnolongergivesanacidreaction.Removeanyundissolvednorbixinbycentrifugationorfiltration,anddrythesolutionoveranhy-droussodiumsulfate.Transfer3to5mLofthedrysolutiontothetopofanaluminacolumnpreparedasdescribedabove.Elutethecolumnwithtoluene,three10-mLvolumesofdryacetone,and5mLofCarr-PriceReagent(seeSolutionsandIndicators)addedtothetopofthecolumn.Theorange-redbandofnorbixinimmediatelyturnsblue-green.ArsenicNotmorethan3mg/kg.ColorIntensityAsamplemeetstherepresentationsofthevendor.LeadNotmorethan10mg/kg.ResidualSolventsAcetone:Notmorethan0.003%;Hex-anes:Notmorethan0.0025%;IsopropylAlcohol:Notmorethan0.005%;MethylAlcohol:Notmorethan0.005%;Trichlo-roethyleneandDichloromethane:Notmorethan0.003%,indi-viduallyorincombination.TESTSArsenicDetermineasdirectedunderArsenicLimitTest,AppendixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds.ColorIntensityOil-SolubleAnnattoExtractsTransferasample,accu-ratelyweighed,intoasolutionof1%glacialaceticacidinacetone,anddilutetoasuitablevolume(absorbanceof0.5to1.0).Filterthesampletoclarifyifnecessary.Measuretheabsorbanceat454nm,andcalculatethecolorintensitybytheformulaA/(b×c),inwhichAistheabsorbanceoftheSampleSolution;bisthelength,incentimeters,ofthecell;andcistheconcentration,ingramsperliter,oftheSampleSolution.Water-SolubleAnnattoExtractsDetermineasdirectedunderOil-SolubleAnnattoExtracts(above),butdissolvethesamplein0.1Msodiumhydroxide,andmeasuretheab-sorbanceat453nm.LeadDetermineasdirectedunderLeadLimitTest,Appen-dixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds,and10goflead(Pb)ioninthecontrol.ResidualSolventsDetermineasdirectedunderResidualSolvent,AppendixVIII.PackagingandStorageStoreunderrefrigerationinfull,well-closedcontainersthataremadefromsteeloraluminumandthataresuitablylined.-Apo-8′-CarotenalApocarotenal;APOHCH3CCH33CH3CHOCHCH33CH3C30H40OFormulawt416.65INS:160eCAS:[1107-26-2]DESCRIPTIONa-Apo-8dark,metallic′-Carotenalsheen.occursItisasfreelyafine,solublecrystallineinchloroformpowderwithandsparinglysolubleinacetone,butitisinsolubleinwater.Itmeltsat136°to140°withdecomposition.FunctionColor.REQUIREMENTSIdentificationA.DeterminetheabsorbanceofSampleSolutionB,pre-paredasdirectedintheAssay(below),at488nmandat460nm.TheratioA488/A460isbetween0.77and0.85.B.DeterminetheabsorbanceofSampleSolutionBat460nm,andthatofSampleSolutionA,preparedasdirectedintheAssay(below),at332nm.TheratioA332/A460isbetween0.63and0.75.AssayNotlessthan96.0%andnotmorethan101.0%ofC30H40O.ArsenicNotmorethan1mg/kg.LeadNotmorethan10mg/kg.ResidueonIgnitionNotmorethan0.2%.TESTSAssay(Note:Carryoutallworkinlow-actinicglasswareandinsubduedlight.)SampleSolutionATransferabout40mgofsample,accu-ratelyweighed,intoa100-mLvolumetricflask,dissolvein10mLofacid-freechloroform,dilutetovolumewithcyclo-hexane,andmix.Pipet2mLofthissolutionintoa50-mLvolumetricflask,dilutetovolumewithcyclohexane,andmix.SampleSolutionBPipet5mLofSampleSolutionAintoa50-mLvolumetricflask,dilutetovolumewithcyclohexane,andmix.ProcedureDeterminetheabsorbanceofSampleSolutionBina1-cmcellatthewavelengthofmaximumabsorption34/Arabinogalactan/Monographs食界论坛http://www.sinofood.com.cn/bbs.htm FCCVatabout460nm,withasuitablespectrophotometer,usingcyclohexaneastheblank.Calculatethequantity,inmilli-grams,ofC30H40Ointhesampletakenbytheformula25,000A/264,inwhichAistheabsorbanceofthesolutionand264istheabsorptivityofpure-Apo-8′-Carotenal.ArsenicDetermineasdirectedunderArsenicLimitTest,AppendixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds.LeadDetermineasdirectedunderLeadLimitTest,Appen-dixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds,and10goflead(Pb)ioninthecontrol.ResidueonIgnitionDetermineasdirectedunderResidueonIgnition,AppendixIIC,ignitinga2-gsample.PackagingandStorageStoreintight,light-resistantcon-tainersunderinertgas.ArabinogalactanLarchFiber;LarchGumINS:409CAS:[9036-66-2]DESCRIPTIONArabinogalactanoccursasawhitetoyellow-white,coarseorfinepowder.ItisthedriedwaterextractfromthewoodofthelarchtreesLarixoccidentalisandLarixlaricina(Fam.Pinaceae).Itisahighlybranchedpolysaccharidethathasamolecularweightof15,000to60,000daltonsandiscomposedofgalactoseunitsandarabinoseunitsintheapproximateratioof6:1.Itisfreelydispersibleinhotorcoldwater.Itisinsolubleinalcohol.FunctionDietaryfiber;humectant;stabilizer.REQUIREMENTSAssay(TotalCarbohydrates)Notlessthan80%ofArabino-galactan.IdentificationAdd20gofsampleto20mLofwater,andstiruntilcompletelydissolved.Pourthesolutionintoa500-mLbeaker,andadd100mLofwater.Transfer7mLoftheresultingsolutioninto250-mLbeakerandadd0.2mLofdilutedleadsubacetateTS.Noprecipitateforms.Add280mLof95%ethylalcoholtotheremainderofthesolution.Aprecipitateforms.Ash(Total)Notmorethan10.0%.LeadNotmorethan0.1mg/kg.InsolubleMatterNotmorethan0.1%.LossonDryingNotmorethan8.0%.ProteinNotmorethan1.0%.StarchPassestest.Carbohydrates(Total)Notlessthan80.0%.TESTSAssay(TotalCarbohydrates)Theremainder,aftersub-tractingfrom100%thesumofthepercentagesofAsh,LossonDrying,andProtein,representsthepercentoftotalcarbo-hydrates(asarabinogalactan)inthesample.Ash(Total)DetermineasdirectedunderAsh(Total),Ap-pendixIIC.LeadDetermineasdirectedforMethodIintheAtomicAbsorptionSpectrophotometricGraphiteFurnaceMethodun-derLeadLimitTest,AppendixIIIB.InsolubleMatterDissolve5gofsampleinabout100mLofwatercontainedina250-mLErlenmeyerflask,add10mLof2.7Nhydrochloricacid,andboilgentlyfor15min.Usesuctiontofilterthehotsolutionthroughatared,filteredcruci-ble;washthoroughlywithhotwater;dryat105°for2h;andweigh.LossonDryingDetermineasdirectedunderLossonDry-ing,AppendixIIC,dryingasampleat105°for5h.ProteinDetermineasdirectedunderNitrogenDetermina-tion,AppendixIIIC,transferringabout3.5gofsample,accu-ratelyweighed,intoa500-mLKjeldahlflask.ThepercentofproteinequalsthepercentofN×6.25.StarchAddafewdropsofiodineTStoa1:10aqueoussolution.Noblueorredcolorappears.PackagingandStorageStoreinwell-closedcontainers.L-ArginineL-2-Amino-5-guanidinovalericAcidNHCH2CH2CH2CCOOHCNHHNH2NH2C6H14N4O2Formulawt174.20CAS:[74-79-3]View IRDESCRIPTIONL-Arginineoccursaswhitecrystalsorasawhitecrystallinepowder.Itissolubleinwater,insolubleinether,andsparinglysolubleinalcohol.Itisstronglyalkaline,anditswatersolu-tionsabsorbcarbondioxidefromtheair.FunctionNutrient.REQUIREMENTSIdentificationTheinfraredabsorptionspectrumofthesam-pleexhibitsrelativemaximaatthesamewavelengthsasthoseofatypicalspectrumasshowninthesectiononInfraredSpectra,usingthesametestconditionsasspecifiedtherein.FCCVMonographs/L-ArginineMonohydrochloride/35食界论坛http://www.sinofood.com.cn/bbs.htm AssayNotlessthan98.5%andnotmorethan101.5%ofC6H14N4O2,calculatedonthedriedbasis.LeadNotmorethan5mg/kg.LossonDryingNotmorethan1.0%.Optical(Specific)Rotation[␣]D20°:Between+27.9°,calculatedonthedriedbasis;or[␣]D25°+26.0°and:Between+25.8°and+27.7°,calculatedonthedriedbasis.ResidueonIgnitionNotmorethan0.2%.TESTSAssayDissolveabout200mgofsample,accuratelyweighed,in3mLofformicacidand50mLofglacialaceticacid,add2dropsofcrystalvioletTS,andtitratewith0.1Nperchloricacidtoagreenendpointoruntilthebluecolordisappearscompletely.Eachmilliliterof0.1Nperchloricacidconsumedintheassayisequivalentto8.710mgofC6H14N4O2.Caution:Handleperchloricacidinanappropriatefumehood.LeadDetermineasdirectedunderLeadLimitTest,Appen-dixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds,and5goflead(Pb)ioninthecontrol.LossonDryingDetermineasdirectedunderLossonDry-ing,AppendixIIC,dryingthesampleat105°for3h.Optical(Specific)RotationDetermineasdirectedunderOptical(Specific)Rotation,AppendixIIB,usingasolutioncontaining8gofapreviouslydriedsampleinsufficient6Nhydrochloricacidtomake100mL.ResidueonIgnitionDetermineasdirectedunderResidueonIgnition,AppendixIIC,ignitinga1-gsample.PackagingandStorageStoreinwell-closed,light-resistantcontainers.L-ArginineMonohydrochlorideL-2-Amino-5-guanidinovalericAcidMonohydrochlorideNHCH2CH2CH2CCOOHCNHHNH2NH2·HClC6H14N4O2·HClFormulawt210.66CAS:[1119-34-2]View IRDESCRIPTIONL-ArginineMonohydrochlorideoccursasawhiteornearlywhitecrystallinepowder.Itissolubleinwater,slightlysolubleinhotalcohol,andinsolubleinether.Itisacidicandmeltswithdecompositionatabout235°.FunctionNutrient.REQUIREMENTSIdentificationTheinfraredabsorptionspectrumofthesam-pleexhibitsrelativemaximaatthesamewavelengthsasthoseofatypicalspectrumasshowninthesectiononInfraredSpectra,usingthesametestconditionsasspecifiedtherein.AssayNotlessthan98.5%andnotmorethan101.5%ofC6H14N4O2·HCl,calculatedonthedriedbasis.LeadNotmorethan5mg/kg.LossonDryingNotmorethan0.3%.Optical(Specific)Rotation[␣]D20°:Between23.5°,calculatedonthedriedbasis;or[␣]D25°+21.3°and:Between21.3°and+23.4°,calculatedonthedriedbasis.ResidueonIgnitionNotmorethan0.1%.TESTSAssayDissolveabout100mgofsample,previouslydriedat105°for3handaccuratelyweighed,in2mLofformicacid,addexactly15.0mLof0.1Nperchloricacid,andheatonawaterbathfor30min.Caution:Handleperchloricacidinanappropriatefumehood.Aftercooling,add45mLofglacialaceticacid,andtitratetheexcessperchloricacidwith0.1Nsodiumacetate,determin-ingtheendpointpotentiometrically.Performablankdetermi-nation(seeGeneralProvisions),andmakeanynecessarycorrection.Eachmilliliterof0.1Nperchloricacidisequivalentto10.53mgofC6H14N4O2·HCl.LeadDetermineasdirectedunderLeadLimitTest,Appen-dixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds,and5goflead(Pb)ioninthecontrol.LossonDryingDetermineasdirectedunderLossonDry-ing,AppendixIIC,dryingthesampleat105°for3h.Optical(Specific)RotationDetermineasdirectedunderOptical(Specific)Rotation,AppendixIIB,usingasolutioncontaining8gofapreviouslydriedsampleinsufficient6Nhydrochloricacidtomake100mL.ResidueonIgnitionDetermineasdirectedunderResidueonIgnition,AppendixIIC,ignitinga1-gsample.PackagingandStorageStoreinwell-closed,light-resistantcontainers.36/AscorbicAcid/Monographs食界论坛http://www.sinofood.com.cn/bbs.htm FCCVAscorbicAcidVitaminC;L-AscorbicAcidOHOHOHHOCH2COOHC6H8O6Formulawt176.13INS:300CAS:[50-81-7]DESCRIPTIONAscorbicAcidoccursaswhiteorslightlyyellowcrystalsoraspowder.Itmeltsatabout190°.Itgraduallydarkensonexposuretolight,isreasonablystableinairwhendry,butrapidlydeterioratesinsolutioninthepresenceofair.Onegramissolubleinabout3mLofwaterandinabout30mLofalcohol.Itisinsolubleinchloroformandinether.FunctionAntioxidant;meat-curingaid;nutrient.REQUIREMENTSIdentificationA.A1:50aqueoussolutionslowlyreducesalkalinecuprictartrateTSat25°,butmorereadilyuponheating.B.Theinfraredabsorptionspectrumofapotassiumbro-midedispersionofthesampleexhibitsmaximaatthesamewavelengthsasthoseofasimilarpreparationofUSPAscorbicAcidReferenceStandard.AssayNotlessthan99.0%andnotmorethan100.5%ofC6H8O6.LeadNotmorethan2mg/kg.Optical(Specific)Rotation[␣]D25°:Between+20.5°and+21.5°.ResidueonIgnitionNotmorethan0.1%.TESTSAssayDissolveabout400mgofsample,accuratelyweighed,inamixtureof100mLofwater,recentlyboiledandcooled,and25mLof2Nsulfuricacid.Titratethesolutionimmediatelywith0.1Niodine,addingstarchTSneartheendpoint.Eachmilliliterof0.1Niodineisequivalentto8.806mgofC6H8O6.LeadDetermineasdirectedintheFlameAtomicAbsorptionSpectrophotometricMethodunderLeadLimitTest,AppendixIIIB,usinga10-gsample.Optical(Specific)RotationDetermineasdirectedunderOptical(Specific)Rotation,AppendixIIB,usingasolutioncontaining1gofsamplein10mLofcarbondioxide-freewater.ResidueonIgnitionDetermineasdirectedunderResidueonIgnition,AppendixIIC,ignitinga2-gsample.PackagingandStorageStoreintight,light-resistantcon-tainers.AscorbylPalmitatePalmitoylL-AscorbicAcidOHOHOHH2COOC(H2C)14H3CCOOHC22H38O7Formulawt414.54INS:304CAS:[137-66-6]DESCRIPTIONAscorbylPalmitateoccursasawhiteoryellow-whitepowder.Itisveryslightlysolubleinwaterandinvegetableoils.Onegramdissolvesinabout4.5mLofalcohol.FunctionAntioxidant.REQUIREMENTSIdentificationA1:10solutioninalcoholdecolorizesdichlo-rophenol–indophenolTS.AssayNotlessthan95.0%ofC22H38O7,calculatedonthedriedbasis.LeadNotmorethan2mg/kg.LossonDryingNotmorethan2%.MeltingRangeBetween107°and117°.Optical(Specific)Rotation[␣]D25°:Between+21°and+24°,calculatedonthedriedbasis.ResidueonIgnitionNotmorethan0.1%.TESTSAssayDissolveabout300mgofsample,accuratelyweighed,in50mLofalcoholcontainedina250-mLErlen-meyerflask,add30mLofwater,andimmediatelytitratewith0.1Niodinetoayellowcolorthatpersistsforatleast30s.Eachmilliliterof0.1Niodineisequivalentto20.73mgofC22H38O7.LeadDetermineasdirectedintheFlameAtomicAbsorptionSpectrophotometricMethodunderLeadLimitTest,AppendixIIIB,usinga10-gsample.LossonDryingDetermineasdirectedunderLossonDry-ing,AppendixIIC,dryingasampleinavacuumovenat560°to600°for1h.MeltingRangeDetermineasdirectedinProcedureforClassIa,underMeltingRangeorTemperature,AppendixIIB.Optical(Specific)RotationDetermineasdirectedunderOptical(Specific)Rotation,AppendixIIB,usingasolutioncontaining1gofsamplein10mLofmethanol.FCCVMonographs/Aspartame/37食界论坛http://www.sinofood.com.cn/bbs.htm ResidueonIgnitionDetermineasdirectedinMethodIunderResidueonIgnition,AppendixIIC,ignitinga2-gsample.PackagingandStorageStoreintightlyclosedcontainers,preferablyinacool,dryplace.L-AsparagineL-␣-AminosuccinamicAcidH2NCOCH2CCOOHHNH2C4H8N2O3Formulawt,anhydrous132.12C4H8N2O3·H2OFormulawt,monohydrate150.13CAS:anhydrous[70-47-3]CAS:monohydrate[5794-13-8]View IRDESCRIPTIONL-Asparagineoccursaswhitecrystalsorasacrystallinepow-der.Itissolubleinwaterandpracticallyinsolubleinalcoholandinether.Itssolutionsareacidtolitmus.Itmeltsatabout234°.FunctionNutrient.REQUIREMENTSIdentificationTheinfraredabsorptionspectrumofthesam-pleexhibitsrelativemaximaatthesamewavelengthsasthoseofatypicalspectrumasshowninthesectiononInfraredSpectra,usingthesametestconditionsasspecifiedtherein.AssayNotlessthan98.0%andnotmorethan101.5%ofC4H8N2O3,calculatedonthedriedbasis.LeadNotmorethan5mg/kg.LossonDryingBetween11.5%Optical(Specific)Rotation[␣]D20°and12.5%.:Between+33.0°and+36.5°,calculatedonthedriedbasis.ResidueonIgnitionNotmorethan0.1%.TESTSAssayDissolveabout130mgofsample,previouslydriedat130°for3handaccuratelyweighed,in3mLofformicacidand50mLofglacialaceticacid,andtitratewith0.1Nperchloricacid,determiningtheendpointpotentiometrically.Caution:Handleperchloricacidinanappropriatefumehood.Performablankdetermination(seeGeneralProvisions),andmakeanynecessarycorrection.Eachmilliliterof0.1Nper-chloricacidisequivalentto13.21mgofC4H8N2O3.LeadDetermineasdirectedunderLeadLimitTest,Appen-dixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds,andusing5goflead(Pb)ioninthecontrol.LossonDryingDetermineasdirectedunderLossonDry-ing,AppendixIIC,dryingasampleat130°for3h.Optical(Specific)RotationDetermineasdirectedunderOptical(Specific)Rotation,AppendixIIB,usingasolutioncontaining10gofapreviouslydriedsampleinsufficient6Nhydrochloricacidtomake100mL.ResidueonIgnitionDetermineasdirectedunderResidueonIgnition,ignitinga1-gsample.PackagingandStorageStoreinwell-closed,light-resistantcontainers.AspartameN-L-␣-Aspartyl-L-phenylalanine1-MethylEster;APMOHOHNOHNHOCH2H3OC14H18N2O5Formulawt294.31INS:951CAS:[22839-47-0]DESCRIPTIONAspartameoccursasawhite,crystallinepowder.Itissparinglysolubleinwaterandslightlysolubleinalcohol.ThepHofa0.8%solutionisbetweenabout4.5and6.0.FunctionSweetener;sugarsubstitute;flavorenhancer.REQUIREMENTSIdentificationTheinfraredabsorptionspectrumofapotas-siumbromidedispersionofsampleexhibitsmaximaonlyatthesamewavelengthsasthoseofasimilarpreparationofUSPAspartameReferenceStandard.AssayNotlessthan98.0%andnotmorethan102.0%ofC14H18N2O5,calculatedonthedriedbasis.5-Benzyl-3,6-dioxo-2-piperazineaceticAcidNotmorethan1.5%.LeadNotmorethan1mg/kg.LossonDryingNotmorethan4.5%.Optical(Specific)Rotation[␣]D20°:Between+14.5°and+16.5°,calculatedonthedriedbasis.OtherRelatedSubstancesNotmorethan2.0%.ResidueonIgnitionNotmorethan0.2%.TESTSAssayTransferabout300mgofsample,accuratelyweighed,toa150-mLbeaker,dissolvein1.5mLof96%38/Aspartame/Monographs食界论坛http://www.sinofood.com.cn/bbs.htm FCCVformicacid,andadd60mLofglacialaceticacid.AddcrystalvioletTS,andtitrateimmediatelywith0.1Nperchloricacidtoagreenendpoint.Caution:Handleperchloricacidinanappropriatefumehood.Note:Use0.1Nperchloricacidpreviouslystandardizedtoagreenendpoint.Ablanktitrationexceeding0.1mLmaybeduetoexcessivewatercontentandmaycauselossofvisualendpointsensitivity.Performablankdetermination(seeGeneralProvisions),andmakeanynecessarycorrection.Eachmilliliterof0.1Nper-chloricacidisequivalentto29.43mgofC14H18N2O5.5-Benzyl-3,6-dioxo-2-piperazineaceticAcidMobilePhaseWeighandtransfer5.6gofpotassiumphosphatemonobasicintoa1-Lflask,add820mLofwater,anddissolve.AdjustthepHto4.3usingphosphoricacid,add180mLofmethanol,andmix.Filterthrougha0.45-mdisk,andde-gas.DilutingSolventAdd200mLofmethanolto1800mLofwater,andmix.ImpurityStandardPreparationTransferabout25mgofUSP5-Benzyl-3,6-dioxo-2-piperazineaceticAcidReferenceStandard,accuratelyweighed,intoa100-mLvolumetricflask.Add10mLofmethanol,anddissolve.Dilutetovolumewithwater,andmix.Pipet15mLofthissolutionintoa50-mLvolumetricflask,dilutetovolumewithDilutingSolvent,andmix.Useafreshlypreparedsolution.SamplePreparationTransferabout50mgofsample,accuratelyweighed,toa10-mLvolumetricflask.DilutetovolumewithDilutingSolvent,andmix.Useafreshlypreparedsolution.ChromatographicSystem(SeeChromatography,Appen-dixIIA.)Useasuitablehigh-performanceliquidchromato-graphequippedwithadetectormeasuringat210nmanda250-×4.6-mm(id)columnpackedwithoctadecylsilanizedsilica(10-mPartisilODS-3,orequivalent),andoperatedunderisocraticconditionsat40°.TheflowrateoftheMobilePhaseisabout2mL/min.SystemSuitabilityThearearesponsesofthreereplicateinjectionsofImpurityStandardPreparationshowarelativestandarddeviationofnotmorethan2.0%.ProcedureSeparatelyinjectequal20-LportionsofIm-purityStandardPreparationandSamplePreparationintothechromatograph,andrecordthechromatograms(theapproxi-materetentiontimeof5-benzyl-3,6-dioxo-2-piperazineaceticacidis4min,andtheapproximateretentiontimeofAspartameis11min).Measurethepeakarearesponseof5-benzyl-3,6-dioxo-2-piperazineaceticacidineachchromatogram.Calcu-latethepercentageof5-benzyl-3,6-dioxo-2-piperazineaceticacidinthesamplebytheformula1000(AUCS)/(ASWU),inwhichAUandASarethepeakarearesponsesof5-benzyl-3,6-dioxo-2-piperazineaceticacidintheSamplePreparationandintheImpurityStandardPreparation,respectively;CSistheconcentration,inmilligramspermilliliter,of5-benzyl-3,6-dioxo-2-piperazineaceticacidintheImpurityStandardPreparation;andWUistheweight,inmilligrams,ofAspar-tametakenfortheSamplePreparation.LeadDetermineasdirectedforMethodIIintheAtomicAbsorptionSpectrophotometricGraphiteFurnaceMethodun-derLeadLimitTest,AppendixIIIB,usinga1-gsample.LossonDryingDetermineasdirectedunderLossonDry-ing,AppendixIIC,dryingasampleat105°for4h.Optical(Specific)RotationDetermineasdirectedunderOptical(Specific)Rotation,AppendixIIB,usingasolutioncontaining4gofsampleinsufficient15Nformicacidtomake100mL.Makethedeterminationwithin30minofpreparingtheSampleSolution.OtherRelatedImpuritiesProceedasdirectedinthetestfor5-Benzyl-3,6-dioxo-2-piperazineaceticAcid(above),ex-ceptusethefollowinginplaceoftheStandardPreparation:OtherRelatedSubstancesStandardPreparationPipet2mLoftheSamplePreparationfromthetestfor5-Benzyl-3,6-dioxo-2-piperazineaceticAcidintoa100-mLvolumetricflask,dilutetovolumewiththeDilutingSolvent,andmix.ProcedureInjectabout20-LportionsoftheOtherRe-latedSubstancesStandardPreparationandtheSamplePrepa-rationintothechromatograph,andrecordthechromatogramforatimeequaltotwicetheretentiontimeofAspartame.InthechromatogramobtainedfromtheSamplePreparation,thesumoftheresponsesofallsecondarypeaks,otherthanthatfor5-benzyl-3,6-dioxo-2-piperazineaceticacid,isnotmorethantheresponseoftheAspartamepeakobtainedinthechromatogramfromtheOtherRelatedSubstancesStandardPreparation.ResidueonIgnitionDetermineasdirectedunderResidueonIgnition,AppendixIIC,ignitinga1-gsample.PackagingandStorageStoreinwell-closedcontainersinacool,dryplace.FCCVMonographs/Aspartame-AcesulfameSalt/39食界论坛http://www.sinofood.com.cn/bbs.htm Aspartame-AcesulfameSaltAPM-Ace;[2-carboxy--(N-(b-methoxycarbonyl-2-phenyl)ethylcarbamoyl)]ethanaminium6-methyl-4-oxo-1,2,3-oxathiazin-3-ide-2,2-dioxide;L-Phenylalanine,L-␣-aspartyl-2-methylestercompoundwith6-methyl-1,2,3-oxathiazin-4(3H)-one2,2-dioxide(1:1)CH2HOOCCH2CHCONHCHCOOCH3NH3NSO2OOCH3C18H23O9N3SFormulawt457.45CAS:[106372-55-8]View IRDESCRIPTIONAspartame-AcesulfameSaltoccursasawhite,crystallinepowder.Itissparinglysolubleinwaterandslightlysolubleinalcohol.FunctionSweetener.REQUIREMENTSIdentificationAninfraredabsorptionspectrumofapotas-siumbromidedispersionofAspartame-AcesulfameSaltex-hibitsmaximaonlyatthesamewavelengthsasthoseofatypicalspectrumasshowninthesectiononInfraredSpectra,usingthesametestconditionsasspecifiedtherein.AssayNotlessthan63.0%andnotmorethan66.0%ofaspartame,calculatedonthedriedbasis.Notlessthan34.0%andnotmorethan37.0%ofacesulfame,calculatedasacidformedonthedriedbasis.5-Benzyl-3,6-dioxo-2-piperazineaceticAcid(DKP)Notmorethan0.5%.LeadNotmorethan1mg/kg.LossonDryingNotmorethan0.5%.Optical(Specific)Rotation[␣]D20°:Between+14.5°and+16.5°,calculatedonthedriedbasis.OtherRelatedImpuritiesNotmorethan1.0%.PotassiumNotmorethan0.5%.TESTSAssay(Note:UseacombinationpH-electrodeforalltitra-tions.)Dissolve0.100to0.150gofsample,accuratelyweighed,in50mLofethanol.Underaflowofnitrogen,titratethesolutionwithstandardized0.1Ntetrabutylammon-iumhydroxideinmethanolor2-propanol.Determinethevol-umeoftitrantneededtoreachthefirstequivalencepoint(V1mL)andthesecondequivalencepoint(V2mL).Performablanktitrationwith50mLofethanol.CalculatethepercentAcesulfameandAspartame,respectively,takenbytheformulas[(V1–VB)×N×163]/(10×W),[(V2–V1)×N×294]/(10×W),inwhichV1,V2,andVBarethenumberofmillilitersof0.1Ntetrabutylammoniumhydroxideinmethanolor2-propanolusedforthesample(firstandsecondequivalencepoints)andtheblank,respectively;Nisthenormalityofthetetrabutylam-moniumhydroxide;Wistheweight,ingrams,ofsampletaken;and163and294aretheformulaweightsofacesulfameandaspartame,respectively.5-Benzyl-3,6-dioxo-2-piperazineaceticAcidMobilePhaseDissolve5.6gofpotassiumphosphate,monobasic,accuratelyweighed,in820mLofwatercontainedina1-Lflask.UsephosphoricacidtoadjustthepHto4.3,add180mLofmethanol,andmix.Filterthrougha0.45-mdisk,andde-gas.DilutingSolventAdd200mLofmethanolto1800mLofwater,andmix.StandardPreparationTransferabout25mgofUSPRef-erenceStandard5-Benzyl-3,6-dioxo-2-piperazineaceticAcid,accuratelyweighed,intoa100-mLvolumetricflask.Add10mLofmethanol,anddissolve.Dilutetovolumewithwater,andmix.Pipet15mLofthissolutionintoa50-mLvolumetricflask,dilutetovolumewiththeDilutingSolvent,andmix.Useafreshlypreparedsolutiononthedayofuse.SamplePreparationTransferabout50mgofsample,accuratelyweighed,intoa10-mLvolumetricflask.DilutetovolumewithDilutingSolvent,andmix.Useafreshlypreparedsolutiononthedayofuse.ChromatographicSystem(SeeChromatography,Appen-dixIIA.)Useasuitablehigh-performanceliquidchromato-graphequippedwithadetectormeasuringat210nmanda250-×4.6-mm(id)columnpackedwithoctadecylsilanizedsilica(10-mPartisilODS-3,orequivalent),andoperatedunderisocraticconditionsat40°.TheflowrateoftheMobilePhaseisabout2mL/min.SystemSuitabilityThearearesponsesofthreereplicateinjectionsoftheStandardPreparationshowarelativestan-darddeviationofnotmorethan2.0%.ProcedureSeparatelyinjectequal20-LportionsoftheStandardPreparationandtheSamplePreparationintothechromatograph,andrecordthechromatograms(theapproxi-materetentiontimeof5-benzyl-3,6-dioxo-2-piperazineaceticacidis4min,andtheapproximateretentiontimeofaspartameis11min).Measurethepeakarearesponseof5-benzyl-3,6-dioxo-2-piperazineaceticacidineachchromatogram.CalculationCalculatethepercent5-benzyl-3,6-dioxo-2-piperazineaceticacidinthesampletakenbytheformula1000×(AUCS)/(ASWU),40/DL-AsparticAcid/Monographs食界论坛http://www.sinofood.com.cn/bbs.htm FCCVinwhichAUandASarethepeakarearesponsesof5-benzyl-3,6-dioxo-2-piperazineaceticacidintheSamplePreparationandintheStandardPreparation,respectively;CSisthecon-centration,inmilligramspermilliliter,of5-benzyl-3,6-dioxo-2-piperazineaceticacidintheStandardPreparation;andWUistheweight,inmilligrams,ofsampletakenfortheSamplePreparation.LeadDetermineasdirectedforMethodIIintheAtomicAbsorptionSpectrophotometricGraphiteFurnaceMethodun-derLeadLimitTest,AppendixIIIB.LossonDryingDetermineasdirectedunderLossonDry-ing,AppendixIIC,dryingasampleat105°for4h.Optical(Specific)RotationDetermineasdirectedunderOptical(Specific)Rotation,AppendixIIB,usingasolutioncontaining6.2gofsampleinsufficient15Nformicacidtomake100mL.Makethedeterminationwithin30minofpreparationoftheSampleSolution.Dividethecalculatedspecificrotationby0.646tocorrectfortheAspartamecontentinAspartame-AcesulfameSalt.OtherRelatedImpuritiesDetermineasdirectedinthetestfor5-Benzyl-3,6-dioxo-2-piperazineaceticAcid(above),butusethefollowingStandardPreparationandProcedure:StandardPreparationPipet1.5mLoftheSamplePrepa-rationfromthetestfor5-Benzyl-3,6-dioxo-2-piperazineaceticAcidintoa100-mLvolumetricflask,dilutetovolumewiththeDilutingSolvent,andmix.ProcedureSeparatelyinjectequal20-LportionsoftheStandardPreparationandtheSamplePreparationintothechromatograph,andrecordthechromatogramsforatimeequaltotwicetheretentiontimeofAspartame.Inthechroma-togramobtainedfromtheSamplePreparation,thesumoftheresponsesofallsecondarypeaks,otherthanthosefor5-benzyl-3,6-dioxo-2-piperazineaceticacidandAcesulfame,isnotmorethantheresponseoftheAspartamepeakobtainedinthechromatogramfromtheStandardPreparation.PotassiumStandardSolutionsTransfer190.7mgofpotassiumchlo-ride,previouslydriedat105°for2h,intoa1000-mLvolumet-ricflask,dilutetovolumewithwater,andmix.Transfer100.0mLofthissolutiontoasecond1000-mLvolumetricflask,dilutetovolumewithwater,andmixtoobtainaStockSolutioncontaining10gofpotassiumpermilliliter(equivalentto19.07gofpotassiumchloride).Pipet10.0-,15.0-,and20.0-mLaliquotsoftheStockSolutionintoseparate100-mLvolu-metricflasks;add2.0mLofa1:5solutionofsodiumchlorideand1.0mLofhydrochloricacidtoeach;dilutewithwatertovolume;andmix.TheStandardSolutionsobtainedcontain,respectively,1.0,1.5,and2.0gofpotassiumpermilliliter.TestSolutionTransferabout3.0gofsample,accuratelyweighed,intoa500-mLvolumetricflask,dilutetovolumewithwater,andmix.Transfer10mLofthissolutionintoa100-mLvolumetricflaskandadd2.0mLofa1:5sodiumchloridesolutionand1.0mLofhydrochloricacid,dilutetovolumewithwater,andmix.Filterthesolution.ProcedureConcomitantlydeterminetheabsorbancesoftheStandardSolutionsandtheTestSolutionatthepotassiumemissionlineof766.5nm,usingasuitableatomicabsorptionspectrophotometerequippedwithapotassiumhollow-cathodelampandanair–acetyleneflame,usingwaterastheblank.PlottheabsorbanceoftheStandardSolutionsversusconcen-tration,inmicrogramspermilliliter,ofpotassium,anddrawthestraightlinebestfittingtheplottedpoints.Fromthegraphsoobtained,determinetheconcentration,C,inmicrogramspermilliliter,ofpotassiumintheTestSolution.Calculatethepercentpotassiuminthesampletakenbytheformula500C/W,inwhichWisthequantity,inmilligrams,ofsampletakentopreparetheTestSolution.PackagingandStorageStoreinwell-closedcontainersinacool,dryplace.DL-AsparticAcidDL-AminosuccinicAcidHOOCCH2CH(NH2)COOHC4H7NO4Formulawt133.10CAS:[617-45-8]View IRDESCRIPTIONDL-AsparticAcidoccursascolorlessorwhitecrystals.Itisslightlysolubleinwater,butinsolubleinalcoholandinether.Itisopticallyinactiveandmeltswithdecompositionatabout280°.FunctionNutrient.REQUIREMENTSIdentificationTheinfraredabsorptionspectrumofthesam-pleexhibitsrelativemaximaatthesamewavelengthsasthoseofatypicalspectrumasshowninthesectiononInfraredSpectra,usingthesametestconditionsasspecifiedtherein.AssayNotlessthan98.5%andnotmorethan101.5%ofC4H7NO4,calculatedonthedriedbasis.LeadNotmorethan5mg/kg.LossonDryingNotmorethan0.3%.ResidueonIgnitionNotmorethan0.1%.TESTSAssayDissolveabout200mgofsample,accuratelyweighed,in3mLofformicacidand50mLofglacialaceticacid,add2dropsofcrystalvioletTS,andtitratewith0.1Nperchloricacidtoagreenendpointoruntilthebluecolordisappearscompletely.Caution:Handleperchloricacidinanappropriatefumehood.FCCVMonographs/Azodicarbonamide/41食界论坛http://www.sinofood.com.cn/bbs.htm Performablankdetermination(seeGeneralProvisions),andmakeanynecessarycorrection.Eachmilliliterof0.1Nper-chloricacidisequivalentto13.31mgofC4H7NO4.LeadDetermineasdirectedunderLeadLimitTest,Appen-dixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds,and5goflead(Pb)ioninthecontrol.LossonDryingDetermineasdirectedunderLossonDry-ing,AppendixIIC,dryingasampleat105°for3h.ResidueonIgnitionDetermineasdirectedunderResidueonIgnition,AppendixIIC,ignitinga1-gsample.PackagingandStorageStoreinwell-closed,light-resistantcontainers.L-AsparticAcidL-AminosuccinicAcidHOOCCH2CCOOHHNH2C4H7NO4Formulawt133.10CAS:[56-84-8]View IRDESCRIPTIONL-AsparticAcidoccursaswhitecrystalsorasacrystallinepowder.Itisslightlysolubleinwater,butinsolubleinalcoholandinether.Itmeltsatabout270°.FunctionNutrient.REQUIREMENTSIdentificationTheinfraredabsorptionspectrumofthesam-pleexhibitsrelativemaximaatthesamewavelengthsasthoseofatypicalspectrumasshowninthesectiononInfraredSpectra,usingthesametestconditionsasspecifiedtherein.AssayNotlessthan98.5%andnotmorethan101.5%ofC4H7NO4,calculatedonthedriedbasis.LeadNotmorethan5mg/kg.LossonDryingNotmorethan0.25%.Optical(Specific)Rotation[␣]D20°:Between+24.5°and+26.0°,calculatedonthedriedbasis.ResidueonIgnitionNotmorethan0.1%.TESTSAssayDissolveabout200mgofsample,accuratelyweighed,in3mLofformicacidand50mLofglacialaceticacid,add2dropsofcrystalvioletTS,andtitratewith0.1Nperchloricacidtoagreenendpointoruntilthebluecolordisappearscompletely.Caution:Handleperchloricacidinanappropriatefumehood.Performablankdetermination(seeGeneralProvisions),andmakeanynecessarycorrection.Eachmilliliterof0.1Nper-chloricacidisequivalentto13.31mgofC4H7NO4.LeadDetermineasdirectedunderLeadLimitTest,Appen-dixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds,and5goflead(Pb)ioninthecontrol.LossonDryingDetermineasdirectedunderLossonDry-ing,AppendixIIC,dryingasampleat105°for3h.Optical(Specific)RotationDetermineasdirectedunderOptical(Specific)Rotation,AppendixIIB,usingasolutioncontaining8gofapreviouslydriedsampleinsufficient6Nhydrochloricacidtomake100mL.ResidueonIgnitionDetermineasdirectedunderResidueonIgnition,AppendixIIC,ignitinga1-gsample.PackagingandStorageStoreinwell-closed,light-resistantcontainers.AzodicarbonamideAzodicarboxylicAcidDiamideOOH2NCNNCNH2C2H4N4O2Formulawt116.08INS:927aCAS:[123-77-3]DESCRIPTIONAzodicarbonamideoccursasayellowtoorange-red,crystal-linepowder.Itispracticallyinsolubleinwaterandinmostorganicsolvents.Itisslightlysolubleindimethylsulfoxide.Itmeltsabove180°withdecomposition.FunctionMaturingagentforflour.REQUIREMENTSIdentificationAsolutionof35mgofsamplein1000mLofwaterexhibitsanultravioletabsorptionmaximumatabout245nm.AssayNotlessthan98.6%andnotmorethan100.5%ofC2H4N4O2afterdrying.LeadNotmorethan5mg/kg.LossonDryingNotmorethan0.5%.NitrogenBetween47.2%and48.7%.pHofa2%SuspensionNotlessthan5.0.ResidueonIgnitionNotmorethan0.15%.TESTSAssayTransferabout225mgofsample,previouslydriedinavacuumovenat50°for2handaccuratelyweighed,into42/BalsamPeruOil/Monographs食界论坛http://www.sinofood.com.cn/bbs.htm FCCVa250-mLglass-stopperediodineflask.Addabout23mLofdimethylsulfoxidetotheflask,washinganyadheredsampledownwiththesolvent,thenstoppertheflask,andplaceabout2mLofthesolventinthecuporlipoftheflask.Swirloccasionally,untilcompletesolutionofthesampleiseffected,andthenloosenthestoppertodraintheremainderofsolventintotheflaskandtorinsedownanydissolvedsampleintothesolution.Add5.0gofpotassiumiodidefollowedby15mLofwater,thenimmediatelypipet10mLof0.5Nhydrochloricacidintotheflask,andrapidlystopper.Swirluntilthepotassiumiodidedissolves,andallowtostandfor20to25minprotectedfromlight.Titratetheliberatediodinewith0.1Nsodiumthiosulfatetothedisappearanceoftheyellowcolor.Titratewithadditionalthiosulfateifanyyellowcolorappearswithin15min.Performablankdetermination(seeGeneralProvisions)onasolutionconsistingof25mLofdimethylsulfoxide,5.0gofpotassiumiodide,15mLofwater,and5mLof0.5Nhydrochloricacid,andmakeanynecessarycorrection.Eachmilliliterof0.1Nsodiumthiosul-fateisequivalentto5.804mgofC2H4N4O2.LeadDetermineasdirectedunderLeadLimitTest,Appen-dixIIIB,usingaSampleSolutionpreparedasdirectedfororganiccompounds,and5gofleadion(Pb)inthecontrol.LossonDryingDetermineasdirectedunderLossonDry-ing,AppendixIIC,dryingasampleinavacuumovenat50°for2h.NitrogenTransferabout50mgofsampleintoa100-mLKjeldahlflask,add3mLofconcentratedhydriodicacidsolu-tion(57%freshlyassayed),anddigestthemixturewithgentleheatingfor1.25h,addingsufficientwater,whennecessary,tomaintaintheoriginalvolume.Increasetheheatattheendofthedigestionperiod,andcontinueheatinguntilthevolumeisreducedbyaboutone-half.Cooltoroomtemperature,add1.5gofpotassiumsulfate,3mLofwater,and4.5mLofsulfuricacid,andheatuntiliodinefumesnolongerevolve.Allowthemixturetocool,washdownthesidesoftheflaskwithwater,heatuntilcharringoccurs,andagaincooltoroomtemperature.Add40mgofmercuricoxidetothecharredmaterial,heatuntilthecolorofthesolutionispaleyellow,thencool,washdownthesidesoftheflaskwithafewmillilitersofwater,anddigestthemixtureforanadditional3h.Coolthedigest,add20mLofammonia-freewater,16mLofa50%sodiumhydroxidesolution,and5mLofa44%sodiumthiosul-fatesolution.ImmediatelyconnecttheflasktoadistillationapparatusasdirectedunderNitrogenDetermination,Appen-dixIIIC,anddistill,collectingthedistillatein10mLofa4%boricacidsolution.Addafewdropsofmethylred–methyleneblueTStothedistillate,andtitratewith0.05Nsulfuricacid.Performablankdetermination(seeGeneralProvisions),andmakeanynecessarycorrection.Eachmillili-terof0.05Nsulfuricacidisequivalentto0.7004mgofnitrogen.pHofa2%SuspensionDetermineasdirectedunderpHDetermination,AppendixIIB,usingthefollowingsolution:Add2gofsampleto100mLofwater,andagitatethemixturewithapowerstirrerfor5min.ResidueonIgnitionDetermineasdirectedunderResidueonIgnition,AppendixIIC,ignitinga1.5-gsample.PackagingandStorageStoreinwell-closed,light-resistantcontainers.BalsamPeruOilCAS:[8007-00-9]View IRDESCRIPTIONBalsamPeruOiloccursasayellowtopalebrown,slightlyviscousliquidhavingasweet,balsamicodor.ItisobtainedbyextractionordistillationofPeruvianBalsamobtainedfromMyroxylonpereiraeRoyleKlotzsche(Fam.Leguminosae).Occasionally,crystalsmayoccurwithintheliquid.Itissolubleinmostfixedoils,andissoluble,withturbidity,inmineraloil.Itispartlysolubleinpropyleneglycol,butitispracticallyinsolubleinglycerin.FunctionFlavoringagent.REQUIREMENTSIdentificationTheinfraredabsorptionspectrumofthesam-pleexhibitsrelativemaximaatthesamewavelengthsasthoseofatypicalspectrumasshowninthesectiononInfraredSpectra,usingthesametestconditionsasspecifiedtherein.AcidValueBetween30and60.AngularRotationBetween–1°and+2°.EsterValueBetween200and225.RefractiveIndexBetween1.567and1.579at20°.SolubilityinAlcoholPassestest.SpecificGravityBetween1.095and1.110.TESTSAcidValueDetermineasdirectedunderAcidValue,Ap-pendixVI.AngularRotationDetermineasdirectedunderOptical(Specific)Rotation,AppendixIIB,usinga100-mmtube.EsterValueDetermineasdirectedinEsterValueunderEsters,AppendixVI,usingabout1gofsample,accuratelyweighed.RefractiveIndexDetermineasdirectedunderRefractiveIndex,AppendixIIB,usinganAbbe´orotherrefractometerofequalorgreateraccuracy.SolubilityinAlcoholDetermineasdirectedunderSolubilityinAlcohol,AppendixVI.Onemilliliterofsampledissolvesin0.5mLof90%alcoholandremainsinsolutionupondilutionto10mL.SpecificGravityDeterminebyanyreliablemethod(seeGeneralProvisions).PackagingandStorageStoreinacoolplaceprotectedfromlightinfull,tightcontainersthataremadefromsteeloraluminumandthataresuitablylined. 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