高效液相色谱法测定血清中的氯硝西泮。

Determination of clonazepam in serum by high performance liquid chromatography.

作者信息

Lin W N

机构信息

Department of Pathology, Henry Ford Hospital, Detroit, Michigan 48202.

出版信息

Ther Drug Monit. 1987 Sep;9(3):337-42. doi: 10.1097/00007691-198709000-00014.

DOI:10.1097/00007691-198709000-00014

PMID:3672578

Abstract

A simple, specific, and sensitive high-performance liquid chromatography (HPLC) method has been developed for the routine monitoring in serum of the benzodiazepine anticonvulsant, clonazepam. Serum spiked with internal standard, methylclonazepam, was vortex-mixed for 1 min with chloroform at an alkaline pH. The evaporated extract was dissolved in the HPLC mobile phase consisting of sodium phosphate buffer, acetonitrile, and methanol. Analytics were resolved at ambient temperature on a 5-micron Supelcosil LC-PCN column (150 X 4.6 mm) equipped with a guard column. Flow rate was 2.0 ml/min, and monitoring was at 306 nm. The calibration curve was linear from 2 to 200 ng/ml. This method provides selectivity and sensitivity with a precision of 3.5%, average recovery of 99%, and no interference from 42 commonly administered drugs.

摘要

已开发出一种简单、特异且灵敏的高效液相色谱（HPLC）方法，用于常规监测血清中的苯二氮䓬类抗惊厥药氯硝西泮。加入内标甲基氯硝西泮的血清在碱性pH条件下与氯仿涡旋混合1分钟。蒸发后的提取物溶解于由磷酸钠缓冲液、乙腈和甲醇组成的HPLC流动相中。分析物在室温下于配备保护柱的5微米Supelcosil LC - PCN柱（150×4.6毫米）上分离。流速为2.0毫升/分钟，监测波长为306纳米。校准曲线在2至200纳克/毫升范围内呈线性。该方法具有选择性和灵敏度，精密度为3.5%，平均回收率为99%，且不受42种常用药物的干扰。