色谱

• 技术与应用 • 上一篇    

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

闫永娜, 王利娟, 杨更亮*, 侯文欣, 张巧霞   

  1. College of Pharmacy of Hebei University, Hebei Province Key Laboratory of Pharmaceutical Quality Control, Baoding 071002, China
  • 收稿日期:2009-07-28 修回日期:2009-09-28 出版日期:2009-11-30 发布日期:1981-12-25
  • 通讯作者: 杨更亮

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

YAN Yongna, WANG Lijuan, YANG Gengliang*, HOU Wenxin, ZHANG Qiaoxia   

  1. College of Pharmacy of Hebei University, Hebei Province Key Laboratory of Pharmaceutical Quality Control, Baoding 071002, China
  • Received:2009-07-28 Revised:2009-09-28 Online:2009-11-30 Published:1981-12-25
  • Contact: YANG Gengliang

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10 kV,运行缓冲液为含有30 mmol/L Brij-35、5%(体积分数)乙腈、0.167 mol/L氯化钠的磷酸二氢钠缓冲液(0.01 mol/L,pH 4.1)。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。

关键词: 多粘菌素E1, 多粘菌素E2, 胶束电动毛细管色谱, 硫酸多粘菌素E

Abstract: 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.

Key words: polymyxin E sulfate , polymyxin E1, polymyxin E2, micellar electrokinetic capillary chromatography (MECC)