USP潑尼松校正片說(shuō)明書(shū)(中英文對(duì)照)

1、Certificate（證書(shū)）PREDNISONETABLETS（潑尼松片）USPCatalogNo.:1559505USPLotNo.:R031Y1（10mgnominalprednisonecontentpertablet）（每片含潑尼松10mg）FORDISSOLUTIONPERFORMANCEVERIFICATIONTEST（PVT）用于溶出性能確認(rèn)實(shí)驗(yàn)Periodofvalidity:ThiscertificateofUSPPrednisoneTabletsLotR031Y1isvalidthroughJune30th,2017.有效期：USP潑尼松片批號(hào)R031Y1的證書(shū)有效期到2

2、017年6月30日TheUSPPrednisoneTabletsRSisprovidedforuseinthePerformanceVerificationTestforUSPApparatus1and2with1litervesselsintheUSPGeneralTestChapteronDISSOLUTION<711>andDRUGRELEASE<724>,APPARATUSSUITABILITY.Storeinadryplace.Storethetabletsatcontrolledroomtemperaturenotexceeding25°.USP潑

3、尼松標(biāo)準(zhǔn)片用于采取USP中方法1和方法2對(duì)1升溶出杯，進(jìn)行USP通用測(cè)試部分溶出（711）和釋放（724）項(xiàng)目的性能能確認(rèn)實(shí)驗(yàn)，藥品貯藏在干燥，溫度低于25°C環(huán)境中。DissolutionMedium:Werecommendpreparingthemediumasfollows:Heatasuitableamountofwater,whilestirringgently,toabout41-45°.Filterundervacuumthrougha0.45-ym-porosityfilterintoasuitablefilteringflaskequippedwithas

4、tirringdevice.Sealtheflaskandcontinuetoapplyvacuumwhilestirringforanadditionalfiveminutes.Measuredvacuumshouldbelessthan100mbar.ThetemperatureoftheDissolutionmediumshouldnotfallbelow37°priortotheinitiationofthetest.溶出介質(zhì)：推薦介質(zhì)準(zhǔn)備（操作）如下：（脫氣純化水）加熱適量水同時(shí)輕輕攪拌到約4145C。真空下用0.45um濾膜過(guò)濾至配有攪拌容器中（即過(guò)濾后需要攪拌），密封容

5、器口并繼續(xù)在真空條件下攪拌5分鐘。檢測(cè)真空度小于100mbar。在實(shí)驗(yàn)開(kāi)始前溶出介質(zhì)溫度不高于37°C。Procedure：SeeDISSOLUTION<711>inthecurrentUSP:Determinethequantityofprednisone,C21H26O5,dissolvedat30minutes,ineachvessel,expressedaspercentofthelabeledamount.Use499gofDissolutionMedium（whichcorrespondsto500mL）,wherepossiblethemediumshoul

6、dnotbestirredpriortotheinitiationofthetestforthepurposeofequilibration,andconductthetestat37°.Operateeachapparatusat50-rpmspeed.Withdrawanaliquotofsamplesolutionat30minutesandfilterimmediately.Measuretheamountofprednisonedissolvedfromfilteredportionsofthesamplealiquotsat242nmincomparisonwithaso

7、lutionofknownconcentrationofUSPPrednisoneReferenceStandard.步驟：查看USP現(xiàn)行版的溶出711：確定潑尼松數(shù)量，每個(gè)溶出杯中溶解30分鐘，結(jié)果用百分比表示。499g溶出介質(zhì)（相當(dāng)于500ml溶出介質(zhì)），為了達(dá)到溶出介質(zhì)平衡，實(shí)驗(yàn)開(kāi)始前不能攪拌溶出介質(zhì)并且溫度控制37Co開(kāi)啟轉(zhuǎn)速50轉(zhuǎn)。30分鐘時(shí)取樣馬上過(guò)濾。在242nm波長(zhǎng)下測(cè)定溶出度（百分比表示）與已知濃度的USP潑尼松參考標(biāo)準(zhǔn)比較。實(shí)驗(yàn)條件：500ml溶岀介質(zhì)、37°C、50轉(zhuǎn)/分鐘、30分鐘取樣檢測(cè)：242nm的波長(zhǎng)下測(cè)定供試品溶液和對(duì)照品溶液的溶出度Note:Anam

8、ountofalcoholnottoexceed5%ofthetotalvolumeofthestandardsolutionmaybeusedtobringtheprednisonereferencestandardintosolution.Thefilteringmethodmustnotcauseabsorptivelossofdrug.Brasintroducedbyautomatedmethodsistobeavoided.Ifequipmentisdedicatedforusewithonlyoneapparatus（basketorpaddie）.thenperformancev

9、erificationisonlyrequiredforthatapparatus.Atthetimeofuse,peelbackthepaper-backedliddingtoremovethetabletsfromtheblistercard注意：1、乙醇的用量應(yīng)不超過(guò)總體積的1。（對(duì)照品先用少量乙醇溶解以加快溶解速度）；2、自動(dòng)取樣系統(tǒng)可以減少偏差；3、如果只儀器只用一種方法（轉(zhuǎn)籃或槳板），僅僅需要對(duì)使用的方法進(jìn)行確認(rèn)；estInterpretation:Laboratorycanchooseeitherofthetestschemeslistedbelow.實(shí)驗(yàn)說(shuō)明：從以下實(shí)驗(yàn)方案中選

10、擇一種Single-StageTest單階實(shí)驗(yàn)：Thefollowingarestep-by-stepinstructionsfortheSingle-Stagetest.單階實(shí)驗(yàn)操作步驟：1. Foreachpositionintheassembly,testoneUSPPrednisoneTabletsRS,andrecordthepercentdissolvedatthesamplingtimepointspecified.Transformthepercentdissolvedresultstothenaturallogscale,determinethemeanandvariance

11、.Forassemblieswith12or14positions（12or14dissolutionvessels）,nofurthertestingisrequired.1每個(gè)溶出杯中放入一粒USP潑尼松片，按照選取方法在規(guī)定時(shí)間點(diǎn)取樣并檢測(cè)溶出度。先將各個(gè)溶出度數(shù)據(jù)計(jì)算得到自然對(duì)數(shù)，再以自然對(duì)數(shù)為數(shù)據(jù)，計(jì)算其平均數(shù)（片1）和方差（81）,12個(gè)和14個(gè)溶出杯的儀器可以不再進(jìn)行后續(xù)檢測(cè)。2. Forassemblieswithfewerthan12positions,repeatStep1withanadditionalsetoftablets.Againaftertransforming

12、thepercentdissolvedresultstothenaturallogscale,determinethemeanandvariance.2. 不到12個(gè)溶出杯的儀器，重復(fù)第1步操作，即再次向每個(gè)溶出杯中放入一粒USP潑尼松片，按照選取方法在規(guī)定時(shí)間點(diǎn)取樣并檢測(cè)溶出度。將檢測(cè)得到的各個(gè)溶出杯結(jié)果計(jì)算平均數(shù)（刃）和方差（82）3. CalculatetheaverageofthetwomeansandofthetwovariancesobtainedinSteps1and2.（UsetheresultsfromStep1aloneforassembliesthathave12or14

13、positions.）3. 將第1、2步中得到的兩個(gè)平均值（片1、%2）和方差（81、82）分別計(jì)算各自的平均值。即文3=論83=81+82，（12個(gè)或者14個(gè)溶出杯無(wú)需計(jì)算，直接取用第1步計(jì)算結(jié)果，2即X3=X1,83=81）24. ConverttheresultsofStep3toageometricmean(GM)andpercentcoefficientofvariation(%CV).Seecalculationexamplebelowformoredetail.4. 第3步中計(jì)算得到的片3和S3按照以下公式計(jì)算得到GM和CV。GM=e無(wú)3%CV=100xJe(S3-i)5. Co

14、mparetheresultsofStep4totheSingleStageacceptancerangesinTable1.TheGMmustnotfalloutsidethelimits,andthe%CVmustnotbegreaterthanthelimit.Ifbothmeetthecriteria,theassemblyhaspassedthePVT.5.第4步計(jì)算得到的GM和%CV結(jié)果與表格1中“SingleStage”項(xiàng)下的相應(yīng)標(biāo)準(zhǔn)比較。GM不能低于范圍下限；%CV需要高于限度標(biāo)準(zhǔn)。如果兩個(gè)結(jié)果均符合標(biāo)準(zhǔn)，性能確認(rèn)通過(guò)。MicrosoftExcel中對(duì)應(yīng)的各個(gè)計(jì)算公式：自然對(duì)數(shù)

15、：LNX:AVERAGES：VAR.Sex:EXP松SQRTOptionalTwo-StageTest：雙階實(shí)驗(yàn)AlaboratorymaychoosetoimplementthePVTasaTwo-Stagetestincaseofassemblieswithlessthan12positions.TheTwo-Stagetestisastatisticallyvalidmeansofallowingthepossibilityofstoppingthetestatthefirststagewithapenalty.Thefollowingarestep-by-stepinstruction

16、sforthetwo-stagetest.出杯數(shù)量小于12個(gè)的情況下，實(shí)驗(yàn)室可以選擇雙階實(shí)驗(yàn)作為性能確認(rèn)。雙階實(shí)驗(yàn)是一個(gè)有效統(tǒng)計(jì)方法允許第一階段(thefirststage)實(shí)驗(yàn)結(jié)果不合格情況下進(jìn)行后續(xù)第二階段實(shí)驗(yàn)(thesecondstage)。操作步驟如下。1. Foreachpositionintheassembly,testoneUSPPrednisoneTabletsRS,andrecordthepercentdissolvedatthesamplingtimepointspecified.Aftertransformingthepercentdissolvedresultstoth

17、enaturallogscale,determinethemeanandvariance.1每個(gè)溶出杯中放入一粒USP潑尼松片，按照選取方法在規(guī)定時(shí)間點(diǎn)取樣并檢測(cè)溶出度。先將各個(gè)溶出度數(shù)據(jù)計(jì)算得到自然對(duì)數(shù)，再以自然對(duì)數(shù)為數(shù)據(jù)，計(jì)算其平均數(shù)（片1）和方差（61）。2. ConverttheresultsofStep1toaGMand%CV,andcomparetothe1stStageofTwoStagesacceptancerangesinTable1.TheGMmustnotfalloutsidethelimits,andthe%CVmustnotbegreaterthanthelimit.

18、ForcalculationoftheGMand%CV,seecalculationexampleformoredetail.2. 第1步中計(jì)算得到的片3和63按照以下公式計(jì)算得到GM和CV。并與表格1中“1stStageofTwoStages”項(xiàng)下的相應(yīng)標(biāo)準(zhǔn)比較。GM不能低于范圍下限；%CV需要高于限度標(biāo)準(zhǔn)。GM=ei%CV=100x7e（6i-i）3. IfresultsofStep2satisfybothacceptancecriteria,theassemblyhaspassedthePVT.OtherwisecontinuetoStep4.（seenote1）.3. 如果第2步兩個(gè)結(jié)

19、果均符合標(biāo)準(zhǔn)，性能確認(rèn)通過(guò)，否則需要繼續(xù)第4步操（見(jiàn)備注1）。4. RepeatStep1withanadditionalsetoftabletsandaftertransformingthepercentdissolvedresultstothenaturallogscaledeterminethemeanandvarianceforthedataobtainedatthisstep.4. 向每個(gè)溶出杯中放入一粒USP潑尼松片，按照選取方法在規(guī)定時(shí)間點(diǎn)取樣并檢測(cè)溶出度。將檢測(cè)得到的各個(gè)溶出杯結(jié)果計(jì)算平均數(shù)（片2）和方差（62）5. Averagethetwomeansandtwovarian

20、cesobtainedinSteps1and4.將第1步和第4步雙階實(shí)驗(yàn)得到的平均值和方差計(jì)算得平均數(shù)兩個(gè)平均值&1、產(chǎn)2）和方差（61、82）分別計(jì)算各自的平均值。81+822即片3=6. ConverttheresultsofStep5toageometricmean(GM)andpercentcoefficientofvariation(%CV).ForcalculationoftheGMand%CV,seecalculationexampleformoredetail.6.第5步中計(jì)算得到的片3和83按照以下公式計(jì)算得到GM和CV。GM=%CV=100xJe(83-i)7. C

21、omparetheresultsofStep6tothe2ndStageofTwoStagesacceptancerangesinTable1.TheGMmustnotfalloutsidethelimits,andthe%CVmustnotbegreaterthanthelimit.Ifbothmeettheacceptancecriteria,theassemblyhaspassedthePVT.第6步計(jì)算得到的GM和%CV結(jié)果與表格1中“2ndStageofTwoStages”項(xiàng)下的相應(yīng)標(biāo)準(zhǔn)比較。GM不能低于范圍下限；%CV需要高于限度標(biāo)準(zhǔn)。如果兩個(gè)結(jié)果均符合標(biāo)準(zhǔn)，性能確認(rèn)通過(guò)。Inor

22、dertocomplywiththerequirementsofASTME29,alllimitvaluesinTable1areexpressedwithtwosignificantfigures.為了滿足ASTME29要求，表格1中標(biāo)準(zhǔn)均用兩位有效數(shù)字標(biāo)示。Table1.PerformanceVerificationTest(PVT)limits(valuesapplyonlytoLotR031Y1)性能確認(rèn)限度標(biāo)準(zhǔn)（批號(hào)R031Y1實(shí)驗(yàn)結(jié)果）Apparatus方法#ofvessels溶出杯數(shù)Single-StageGM*%CV1654-841178Two-Stage1stStageofT

23、woStages2ndStageofTwoStagesGM*%CVGM*%CV58-808.254-841112142627-406.476.386.2126.3146.2nana29-364.727-406.34.86.2nana*Percentofthelabeledamountofprednisonedissolvedat30minutesat50-rpmCalculationexample(expressedasMicrosoftExcelworksheetfunctions):Run1:x1,x2,.,xninnaturallogscale:Lnx1,Lnx2,LnxnRun2:xn+1,xn+2,.,x2ninnaturallogscale:Lnxn+1,Lnxn+2,Lnx2n1stStageofTwo-Stageforn=6,7,8andSingle-Stageforn=12,14:GM1=exp(average(Lnx1:Lnxn)%CV1=100*sqrt(exp(var(Lnx1:Lnxn)-1)Single-Stageor2ndStageofTwo-Stagefo