摘要
目的利用HPLC色谱杂质谱对头孢西酮钠中杂质进行定量分析和利用液质联用法初步推断主要杂质结构。方法采用18烷基硅烷键合硅胶为填充剂,以磷酸盐缓冲液(50 mmol·L^(-1)磷酸水溶液,用三乙胺调p H4.0)-乙腈(体积比为85∶15)为流动相,检测波长278 nm,流速1.0 m L·min^(-1),柱温35℃,进样量10μL,检测头孢西酮钠杂质谱;通过HPLC-MS初步鉴定杂质。分别用自身对照法和系统指纹定量法对统一化杂质谱的杂质数目和分布情况以及杂质总含量进行评价。结果根据头孢西酮钠合成路线和HPLC-MS测定结果初步推断5个杂质的可能结构,并测定11个杂质含量。用系统指纹定量法对杂质谱的杂质数目和分布情况及杂质总含量的评价结果基本反应了杂质总量情况。结论系统指纹定量法对杂质数目和含量分布情况及杂质总量评价具有快速便捷的特点,《药物杂质谱数字化定量评价系统》5.0软件能快速计算杂质含量。
Objective To determine the contents of the impurities in cefazedone sodium by HPLC impurity profiles and primarily infer the structures of the main impurities by HPLC-MS. Methods The operation as carried out using an octadecylsilane bonded silica as a solid phase,with the mobile phase consisting of a mixture of phosphate buffer（ 50 mmol·L^-1 aqueous solution of phosphoric acid,then adjusted to p H 4. 0w ith triethylamine）-acetonitrile（ V ∶ V = 85 ∶ 15）. The detection avelength as set at 278 nm,the flow rate as 1. 0 m L·min^-1,the column temperatureas（ 35. 00 ± 0. 15） ℃ and the injection volumeas 10 μL.Then the impurity profiles of cefazedone sodium ere detected,and preliminary identification of impurities as achieved by HPLC-MS. Finally,the quantity,distribution in the content for all impurities in the unified impurity profiles ere evaluated by self-control method and systematically quantified fingerprint method（ SQFM）,respectively. Results According to cefazedone sodium＇s synthetic route and HPLC-MS results,the possible structures of five impurities ere identified and the contents of 11 impurities ere determined. The results of the quantity,distribution in the content for all impurities ere assessed by SQFM,for hich ere basically reflect the total content of the impurities. Conclusions SQFMprovides a rapidly and briefly strategy for assessing the quantity,distribution in the content for all impurities and the total content and ＂Quantitative Evaluation of Digital Control System for Medicine Impurity Profile＂5. 0 softw are can fast calculate the total content of the impurities.
出处
《沈阳药科大学学报》
CAS
CSCD
北大核心
2016年第8期622-626,共5页
Journal of Shenyang Pharmaceutical University
基金
国家基础科学人才培养基金资助项目(J1103606)
