采用固相（Bond-Elut）萃取法对人血清中氯硝西泮进行液相色谱分析。

Liquid chromatographic analysis of clonazepam in human serum with solid-phase (Bond-Elut) extraction.

作者信息

Kabra P M, Nzekwe E U

出版信息

J Chromatogr. 1985 Jun 14;341(2):383-90. doi: 10.1016/s0378-4347(00)84051-7.

Abstract

A simple, sensitive, selective and precise liquid-column chromatographic assay for clonazepam is described, in which 1 ml of serum containing 50 micrograms/l methylclonazepam as an internal standard is extracted by elution from a Bond-Elut column with 400 microliter of methanol. An aliquot of the eluate is injected on to a reversed-phase column and eluted with a mobile phase of acetonitrile--phosphate buffer (30:70) at a flow-rate of 2 ml/min at a column temperature of 50 degrees C. Detection is at 254 nm. Chromatography is complete in 12 min. A sensitivity of 2 ng/ml is attained when 1 ml of serum is extracted. Analytical recovery of the clonazepam added to serum ranged from 91% to 99% with a coefficient of variation of 6.0%. This assay for clonazepam has good precision, with coefficients of variation of 11% at 15 ng/ml and 2.6% at 50 ng/ml. There was no interference from any of the commonly used antiepileptics.

摘要

本文描述了一种用于氯硝西泮的简单、灵敏、选择性好且精确的液相柱色谱分析方法。取1 ml含50 μg/l甲基氯硝西泮作为内标的血清，用400 μl甲醇从Bond-Elut柱上洗脱提取。取部分洗脱液注入反相柱，在柱温50℃下，以2 ml/min的流速用乙腈 - 磷酸盐缓冲液（30:70）作为流动相进行洗脱。检测波长为254 nm。12分钟内完成色谱分析。提取1 ml血清时，检测灵敏度可达2 ng/ml。添加到血清中的氯硝西泮的分析回收率在91%至99%之间，变异系数为6.0%。该氯硝西泮分析方法精密度良好，15 ng/ml时变异系数为11%，50 ng/ml时变异系数为2.6%。常用的抗癫痫药物均无干扰。