欧洲药典对乙酰氨基酚原料质量标准——有关物质检测(译文).docx

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1、EP检测方法：Relatedsubstances.Liquidchromatography(2.2.29).Preparethesolutionsimmediatelybeforeuse.Testsolution.Dissolve0.200gofthesubstancetobeexaminedin2.5mLofmethanolRcontaining4.6g/Lofa400g/LsolutionoftetrabutylammoniumhydroxideRanddiluteto10.0mLwithamixtureofequalvolumesofa17.9g/L

2、solutionofdisodiumhydrogenphosphateRandofa7.8g/LsolutionofsodiumdihydrogenphosphateR.Referencesolution(a).Dilute1.0mLofthetestsolutionto50.0mLwiththemobilephase.Dilute5.0mLofthissolutionto100.0mLwiththemobilephase.Referencesolution(b).Dilute1.0mLofreferencesolution(a)to10.0mLwitht

3、hemobilephase.Referencesolution(c).Dissolve5.0mgof4-aminophenolR,5mgofparacetamolCRSand5.0mgofchloroacetanilideRinmethanolRanddiluteto20.0mLwiththesamesolvent.Dilute1.0mLto250.0mLwiththemobilephase.Referencesolution(d).Dissolve20.0mgof4-nitrophenolRinmethanolRanddiluteto50.0mLwith

4、thesamesolvent.Dilute1.0mLto20.0mLwiththemobilephase.有关物质。液相色谱(2.2.29)。溶液临用现配。供试品溶液：取0.200g的物质溶解在2.5ml甲醇溶液(含有400g/L的氢氧化四丁铵溶液4.6g/L)中，再用17.9g/L的磷酸氢二钠溶液和7.8g/L磷酸二氢钠溶液的等体积混合液稀释至10ml。对照溶液A：取供试品溶液1.0ml用流动相稀释至50ml，再取该溶液5.0ml稀释至100.0ml。对照溶液B：取对照溶液A1.0ml用流动相稀释至10ml。对照溶液C：取5.0mg4-aminophen

5、ol对照品,5mgparacetamolCRS对照品和5.0mgchloroacetanilide对照品用甲醇溶解并稀释到20.0ml。取1.0ml用流动相稀释至250.0ml。对照溶液D：取20.0mg4-nitrophenol对照品用甲醇溶解和稀释到50.0ml。取1ml用流动相稀释至20ml。Column:—size:l=0.25m,Ø=4.6mm,—stationaryphase:octylsilylsilicagelforchromatographyR(5μm),—temperature:35°C.Mobilephase:mix375volume

6、sofa17.9g/LsolutionofdisodiumhydrogenphosphateR,375volumesofa7.8g/LsolutionofsodiumdihydrogenphosphateRand250volumesofmethanolRcontaining4.6g/Lofa400g/LsolutionoftetrabutylammoniumhydroxideR.Flowrate:1.5mL/min.Detection:spectrophotometerat245nm.Injection:20μL.Runtime:12timestheret

7、entiontimeofparacetamol.Relativeretentionswithreferencetoparacetamol(retentiontime=about4min):impurityK=about0.8;impurityF=about3;impurityJ=about7.色谱柱:C-8色谱柱250mm*4.6mm*5μm柱温:35°C。流动相:17.9g/L磷酸氢二钠:7.8g/L的磷酸二氢钠溶液:甲醇溶液(含400g/L的四丁基氢氧化铵4.6g/L)=375:375:250。流量:1.5毫升/分钟。检测波长245nm。进样量:20μ

8、L。运行时间:12倍扑热息痛的保留时间。相对保留（参照对乙酰氨基酚