USP辅料标准.docx
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USP辅料标准.docx
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USP辅料标准
Talc
»Talcisapowdered,selected,natural,hydratedmagnesiumsilicate.PuretalchastheformulaMg3Si4O10(OH)2.Itmaycontainvariableamountsofassociatedmineralsamongwhichchlorites(hydratedaluminumandmagnesiumsilicates),magnesite(magnesiumcarbonate),calcite(calciumcarbonate),anddolomite(calciumandmagnesiumcarbonate)arepredominant.
Labeling—Thelabelstates,whereapplicable,thatthesubstanceissuitablefororalortopicaladministration.Thecertificateofanalysisstatestheabsenceofasbestos.ItalsoindicateswhichmethodspecifiedunderthetestforAbsenceofasbestoswasusedforanalysis.
Identification—
A:
TheIRspectrumofapotassiumbromidedispersionofitexhibitsmaximaat3677±2cm–1,at1018±2cm–1,andat669±2cm–1.
B:
Mixabout200mgofanhydroussodiumcarbonatewith2gofanhydrouspotassiumcarbonate,andmeltinaplatinumcrucible.Tothemeltadd100mgofthesubstanceundertest,andcontinueheatinguntilfusioniscomplete.Cool,andtransferthefusedmixturetoadishorbeakerwiththeaidofabout50mLofhotwater.Addhydrochloricacidtotheliquiduntileffervescenceceases,thenadd10mLmoreoftheacid,andevaporatethemixtureonasteambathtodryness.Cool,add20mLofwater,boil,andfilterthemixture:
[NOTE—SavetheinsolubleresidueforuseinIdentificationtestC.]To5mLofthefiltrateadd1mLof6Nammoniumhydroxideand1mLofammoniumchlorideTS.Filter,ifnecessary,andadd1mLofdibasicsodiumphosphateTStothefiltrate:
awhitecrystallineprecipitateofmagnesiumammoniumphosphateisformed.
C:
Inaleadorplatinumcrucibleandusingacopperwire,mixabout100mgoftheinsolubleresidueasobtainedinIdentificationtestBwithabout10mgofsodiumfluorideandafewdropsofsulfuricacidtogiveathinslurry.Coverthecruciblewithathintransparentplateofplasticunderwhichadropofwaterissuspended,andwarmgently.Withinashorttime,awhiteringisrapidlyformedaroundthedropofwater.
Microbiallimits
61
—Ifintendedfortopicaladministration,thetotalaerobicmicrobialcountdoesnotexceed100cfuperg,andthetotalcombinedmoldsandyeastscountdoesnotexceed50cfuperg.Ifintendedfororaladministration,thetotalaerobicmicrobialcountdoesnotexceed1000cfuperg,andthetotalcombinedmoldsandyeastscountdoesnotexceed100cfuperg.
Acidityandalkalinity—Boil2.5gofTalcwith50mLofcarbondioxide-freewaterunderreflux.Filterundervaccum.To10mLofthefiltrate,add0.1mLof
bromothymolblueTS.Notmorethan0.4mLof0.01Nhydrochloricacidisrequiredtochangethecoloroftheindicator.To10mLofthefiltrate,add0.1mLofphenolphthaleinTS:
notmorethan0.3mLof0.01Nsodiumhydroxideisrequiredtochangethecoloroftheindicatortopink.
Lossonignition
733
—Weighaccuratelyabout1gandigniteat1075±25
toconstantweight:
itlosesnotmorethan7.0%ofitsweight.
Water-solublesubstances—To10.0gadd50mLofcarbondioxide-freewater,heattoboiling,andboilunderarefluxcondenserfor30minutes.Allowtocool,filter,anddilutewithcarbondioxide-freewaterto50.0mL:
thefiltrateisneutraltolitmuspaper.Evaporate25.0mLofthefiltratetodryness,anddryat105
for1hour:
theweightoftheresiduedoesnotexceed5mg(0.1%).
Limitofiron—
Teststocksolution—Weigh10.0gofTalcintoaconicalflaskfittedwitharefluxcondenser,graduallyadd50mLof0.5Nhydrochloricacidwhilestirring,andheatonawaterbathfor30minutes.Allowtocool.Transferthemixturetoabeaker,andallowtheundissolvedmaterialtosettle.Filterthesupernatantintoa100-mLvolumetricflask,retainingasmuchaspossibleoftheinsolublematerialinthebeaker.Washtheresidueandthebeakerwiththree10-mLportionsofhotwater.Washthefilterwith15mLofhotwater,allowthefiltratetocool,anddilutewithwaterto100.0mL.
Testsolution—Transfer2.5mLoftheTeststocksolutiontoa100-mLvolumetricflask,add50.0mLof0.5Nhydrochloricacid,anddilutewithwatertovolume.
Standardironstocksolution—Transfer863.4mgofferricammoniumsulfatetoa100-mLvolumetricflask,dissolveinwater,add10mLof2Nsulfuricacid,anddilutewithwatertovolume.Pipet25mLofthissolutionintoa100-mLvolumetricflask,add10mLof2Nsulfuricacid,dilutewithwatertovolume,andmix.Thissolutioncontainstheequivalentof250µgofironpermL.
Standardironsolutions—Intofour100-mLvolumetricflasks,eachcontaining50.0mLof0.5Nhydrochloricacid,transferrespectively2.0,2.5,3.0,and4.0mLoftheStandardironstocksolution,anddiluteeachflaskwithwatertovolume.
Procedure—ConcomitantlydeterminetheabsorbanceoftheTestsolutionandtheStandardironsolutionsattheironemissionlineof248.3nmwithanatomicabsorptionspectrophotometer(seeSpectrophotometryandLight-Scattering
851
)equippedwithanironhollow-cathodelampandanair–acetyleneflame.Makeanycorrectionusingadeuteriumlamp:
notmorethan0.25%ofironisfound.
Limitoflead—
Testsolution—UsetheTeststocksolution,preparedasdirectedinthetestforLimitofiron.
Leadstandardstocksolution—Dissolve160mgofleadnitratein100mLwaterthatcontains1mLofnitricacid,anddilutewithwaterto1000mL.Pipet10mLofthissolutionintoa100-mLvolumetricflask,dilutewithwatertovolume,andmix.Thissolutioncontainstheequivalentof10µgofleadpermL.
Standardleadsolutions—Intofouridentical100-mLvolumetricflasks,eachcontaining50.0mLof0.5Nhydrochloricacidtransferrespectively5.0,7.5,10.0,and12.5mLofLeadstandardstocksolution,anddilutewithwatertovolume.
Procedure—ConcomitantlydeterminetheabsorbanceoftheTestsolutionandtheStandardleadsolutionsattheleademissionlineof217.0nmwithanatomicabsorptionspectrophotometer(seeSpectrophotometryandLight-Scattering
851
)equippedwithaleadhollow-cathodelampandanair–acetyleneflame:
notmorethan0.001%ofleadisfound.
Limitofcalcium—
Cesiumchloridesolution—Dissolve2.53gofcesiumchloridein100mLofwater,andmix.
Lanthanumchloridesolution—To5.9goflanthanumoxideslowlyadd10mLofhydrochloricacid,andheattoboiling.Allowtocool,anddilutewithwaterto100mL.
Teststocksolution—[Caution—Perchloratesmixedwithheavymetalsareknowntobeexplosive.Takeproperprecautionswhileperformingthisprocedure.]Weigh500mgofTalcina100-mLpolytetrafluoroethylenedish,add5mLofhydrochloricacid,5mLoflead-freenitricacid,and5mLofperchloricacid.Stirgently,thenadd35mLofhydrofluoricacid,andevaporateslowlyonahotplatetomoistdryness(untilabout0.5mLremains).Totheresidue,add5mLofhydrochloricacid,coverwithawatchglass,heattoboiling,andallowtocool.Rinsethewatchglassandthedishwithwater,andtransferintoa50-mLvolumetricflaskcontaining5mLoftheCesiumchloridesolution.Rinsethedishagainwithwater,anddilutewithwatertovolume.
Testsolution—Transfer5.0mLoftheTeststocksolutiontoa100-mLvolumetricflask,add10.0mLofhydrochloricacidand10mLofLanthanumchloridesolution,anddilutewithwatertovolume.
Calciumstandardstocksolution—Dissolve3.67gofcalciumchloridedihydrateindilutedhydrochloricacid,anddilutewiththesamesolventto1000mL.Immediatelybeforeuse,pipet10mLofthissolutionintoa100-mLvolumetricflask,dilutewithwatertovolume,andmix.Thissolutioncontainstheequivalentof100µgofcalciumpermL.
Standardcalciumsolutions—Intofouridentical100-mLvolumetricflasks,eachcontaining10.0mLofhydrochloricacidand10mLofLanthanumchloridesolution,transferrespectively1.0,2.0,3.0,and4.0mLofCalciumstandardstocksolution,anddiluteeachflaskwithwatertovolume.
Procedure—ConcomitantlydeterminetheabsorbanceoftheTestsolutionandtheStandardcalciumsolutionsatthecalciumemissionlineof422.7nmwithanatomicabsorptionspectrophotometer(seeSpectrophotometryandLight-Scattering
851
)equippedwithacalciumhollow-cathodelampandanitrousoxide–acetyleneflame:
notmorethan0.9%ofcalciumisfound.
Limitofaluminum—
CesiumchloridesolutionandTeststocksolution—ProceedasdirectedinthetestforLimitofcalcium.
Testsolution—Transfer5.0mLoftheTeststocksolutiontoa100-mLvolumetricflask,add10mLoftheCesiumchloridesolutionand10.0mLofhydrochloricacid,anddilutewithwatertovolume.
Aluminumstandardstocksolution—Dissolve8.947gofaluminumchlorideinwater,anddilutewithwaterto1000mL.Immediatelybeforeuse,pipet10mLofthissolutionintoa100-mLvolumetricflask,dilutewithwatertovolume,andmix.Thissolutioncontainstheequivalentof100µgofaluminumpermL.
Standardaluminumsolutions—Intofouridentical100-mLvolumetricflasks,eachcontaining10.0mLofhydrochloricacidand10mLofCesiumchloridesolution,transferrespectively5.0,10.0,15.0,and20.0mLofAluminumstandardstocksolution,anddilutewithwatertovolume.
Procedure—ConcomitantlydeterminetheabsorbanceoftheTestsolutionandtheStandardaluminumsolutionsatthealuminumemissionlineof309.3nmwithanatomicabsorptionspectrophotometer(seeSpectrophotometryandLight-Scattering
851
)equippedwithanaluminumhollow-cathodelampandanitrousoxide–acetyleneflame:
notmorethan2.0%ofaluminumisfound.
Absenceofasbestos—[NOTE—SuppliersofTalcmayuseoneofthefollowingmethodstodeterminetheabsenceofasbestos.]ProceedasdirectedfortestAortestB.Ifeithertestispositive,perform
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