弱离子交换整体柱在线预处理并测定人尿液中头孢唑啉钠
Weak Ion Exchange Monolithic Column for On-Line Clean- Up and Determination of Cefazolin Sodium in Human Urine
用乙二胺将以甲基丙烯酸缩水甘油酯(GMA), 甲基丙烯酸(MAA)为单体,乙二醇二甲基丙烯酸酯(EDMA)为交联剂的整体柱在线修饰为弱离子交换整体柱(包括羧基和乙二胺基两种离子交换基团)作预处理介质,水下可以去除人尿液和血浆中的大分子干扰物质,同时对带负电荷的小分子药物有富集作用,本文用该离子柱在线预处理同时测定人尿液中头孢唑啉钠。分析流动相为9.4 mM Na2HPO4 和5.3 mM 柠檬酸-乙腈(体积比87:13),流速为1mL/min, 在254 nm处进行检测。头孢唑啉尿样在1.0-100µg/mL范围内线性关系良好,头孢唑啉在尿样中平均回收率为98.8±3.0%,最低检出限为0.3µg/mL,结果表明用该弱离子交换整体柱可进行简单,快速的在线样品处理。
weak ion exchange monolithic column prepared by modifying the GMA-MAA-EDMA (glycidyl methacrylate-methacrylic acid-ethylene glycol dimethacrylate) monoliths with ethylenediamine was applied to remove matrix compounds in biological fluid that otherwise would interfere with the analysis. Water could be used as the washing liquid to flush out matrix compounds while retaining negative charged small molecules. Using this monolithic column, on-line clean-up and screening of cefazolin sodium in human urine samples had been investigated. Chromatography was performed by reversed-phase HPLC on a C18 column with ultraviolet detection at 254nm. The mobile phase was an aqueous solution containing 9.4 mM Na2HPO4 and 5.3 mM citric acid with acetonitrile (87:13 V/V). Calibration curve was linear in the concentration range of 1.0-100µg/mL for cefazolin in human urine The mean recovery was 98.8±3.0% and the LOQ was 0.3µg/mL. Results showed that the weak ion exchange monolithic column could be used for deproteinization and retaining cefazolin sodium in human urine, which provided a simple and fast method for assaying drugs in human urine and plasma.
冯莎、尹俊发、杨更亮、张骊、刘海燕、蔡丽萍
药学生物科学研究方法、生物科学研究技术
头孢唑啉钠在线样品处理弱离子交换整体柱
efazolin SodiumOn-line sample clean- upWeak ion exchange monolithic column
冯莎,尹俊发,杨更亮,张骊,刘海燕,蔡丽萍.弱离子交换整体柱在线预处理并测定人尿液中头孢唑啉钠[EB/OL].(2007-01-25)[2025-08-21].http://www.paper.edu.cn/releasepaper/content/200701-361.点此复制
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