胶束电动毛细管色谱法测定硫酸多粘菌素E药物中的多粘菌素E1和E2  

Determination of polymyxin E1 and polymyxin E2 in polymyxin E sulfate using micellar electrokinetic capillary chromatography

作　　者：闫永娜[1] 王利娟[1] 杨更亮[1] 侯文欣[1] 张巧霞[1] 

机构地区：[1]河北大学药学院,河北省药物质量分析控制重点实验室,河北保定071002

出　　处：《色谱》2009年第6期860-863,共4页Chinese Journal of Chromatography

基　　金：国家自然科学基金项目(Nos.20375010,20675084);河北省科技攻关项目(Nos.06276479D,07276407D);河北省教育厅项目(No.Z2007225)

摘　　要：采用胶束电动毛细管色谱法(MECC)对硫酸多粘菌素E药物中的主要成分多粘菌素E1和E2进行了分离,并测定了多粘菌素E1、E2的含量。分别考察了电泳电压、表面活性剂种类、Brij-35(月桂醇聚氧乙烯醚)浓度、乙腈含量、磷酸盐缓冲液的pH值、氯化钠浓度等实验参数对实验结果的影响,从而确定了最佳的分离条件:电泳电压为10kV,运行缓冲液为含有30mmol/L Brij-35、5%(体积分数)乙腈、0.167mol/L氯化钠的磷酸二氢钠缓冲液(0.01mol/L,pH4.1)。在优化的实验条件下,E1和E2得到了较好的分离,分离度达到1.94。以多粘菌素E1为例,柱效和峰面积的日间及日内测定的相对标准偏差(RSD)均小于5%。E1和E2在硫酸多粘菌素E药物中的含量分别为67%和32%。该方法简便、快速、准确、重现性好。A method of micellar electrokinetic chromatography capillary （MECC） has been established for separating polymyxins E1 and E2 in polymyxin E sulfate and determining the contents of E1 and E2. Several factors including the running voltage, the type of surfactant, concentrations of Brij-35 （polyoxyethyleneglycol dodecyl ether）, NaCl solution and acetonitrile, pH of phosphate were investigated. Under the optimum conditions （ 10 kV running voltage, phosphate buffer solution （0.01 mol/L, pH 4. 1 ） containing 30 mmol/L Brij-35, 5% （v/v） acetonitrile, 0. 167 mol/L NaCl）, E1 and E2 were separated with the resolution of 1. 94. The contents of E1 and E2 in polymyxin E sulfate were 67% and 32%, respectively. As an example, the relative standard deviations of the intra-assay and inter-assay of polymyxin E1 on the plate number and peak area were less than 5%. The method is simple, rapid, accurate, and reproducible.

关 键 词：胶束电动毛细管色谱 多粘菌素E1 多粘菌素E2 硫酸多粘菌素E 

分 类 号：O658[理学—分析化学]