摘要
目的:探讨对头孢氨苄、头孢拉定原料中增加2-萘酚检查的必要性,建立科学、合理的2-萘酚检查方法以及限度。方法:采用HPLC-UV法,C18(4.6 mm×250 mm,5μm)色谱柱,以甲醇-水(55∶45)为流动相,流速为1.0 mL.min-1;检测波长为225 nm,分析20批头孢氨苄原料、2批头孢拉定原料以及217批头孢氨苄片(胶囊)、380批头孢拉定胶囊中含2-萘酚的量,并进行方法学验证。结果:方法专属性强、线性范围宽、精密度好、准确度高、耐用性好,超过50%的样品含有不同量的2-萘酚,有些企业样品中含量较大,同一企业样品批间差异较大;根据当前ICH指导原则以及已发表的文献资料,初步确定了头孢氨苄、头孢拉定原料中2-萘酚的限度。结论:建议在中国药典头孢氨苄、头孢拉定原料中增加2-萘酚检查项并初步拟定了限度,其限度科学性、合理性需进一步验证。
Objective：To disscuss the necessity for establishing the quality control method for determining 2-naphthol in cefalexin and cefradine raw substance and building a scientific and reseanable test method and specification limit for 2-naphthol.Methods：Analyzed the content of 2-naphthol in 20 lots of cefalexin raw substance,2 lots of cefradine raw substance,217 lots of cefalexin tablets/capsule and 380 lots of cefradine capsules using by a HPLC-UV method which was equipped with a C18（4.6 mm×250 mm,5 μm） column and using a mixture of methanol-water（55：45） as mobile phase and the flow rate was 1.0 mL·min-1 and the detection wavelength was 225 nm.The method was validated adequeatly.Results：The HPLC method is specific,linear,accurate,precise and robust.More than 50% medicine samples（drug substance and drug product）contain different content of 2-naphthol and some samples contain a great quantity of 2-naphthol.There were significant differences between different batches from the same company.The specification limits of 2-naphthol in cefalexin and cefradine drug substance monograph were initially built according to the current ICH guidelines and published literatures.Conclusions：Suggestion establishing the control method for determining 2-naphthol in cefalexin and cefradine drug substance in Chinese Pharmacophia monograph containing the specification limits which need more validating scientifically and reseanably by future literatures.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2012年第4期555-565,共11页
Chinese Journal of Pharmaceutical Analysis
基金
国家科技重大专项课题"微生物药物技术创新与新药创制产学研联盟"(No.2010ZX09401-403)资助
