马钱子及其制剂中士的宁和马钱子碱的非水毛细管电泳分离与测定

Separation and determination of strychnine and brucine in Strychnos nux-vomica L. and its preparation by nonaqueous capillary electrophoresis.

作者信息

Li Yuqin, He Xiaojun, Qi Shengda, Gao Wenhua, Chen Xingguo, Hu Zhide

机构信息

Department of Chemistry, Lanzhou University, Lanzhou 730000, PR China.

出版信息

J Pharm Biomed Anal. 2006 May 3;41(2):400-7. doi: 10.1016/j.jpba.2005.11.036. Epub 2006 Jan 9.

DOI:10.1016/j.jpba.2005.11.036

PMID:16406713

Abstract

An easy, rapid method for simultaneous determination of strychnine and brucine in Strychnos nux-vomica L. and its preparation was developed by nonaqueous capillary electrophoresis (NACE) without pretreatment for the first time. Optimum separation was achieved with a fused-silica capillary column (50 cmx75 microm i.d.) and a running buffer containing 30 mM ammonium acetate, 1.0% acetic acid and 15% acetonitrile (ACN) in methanol medium. The applied voltage was 30.0 kV. The analytes were detected by UV at 214 nm. The effects of concentration of ammonium acetate, acetic acid and organic modifier on electrophoretic behavior of the analytes were studied. The established method with sophoridine as internal standard was linear in the range of 5-1000 mg/mL for both strychnine and brucine. The extracts of Strychnos nux-vomica and its preparation could be directly injected for determination with recoveries ranging from 94.5 to 104%.

摘要

首次开发了一种简便、快速的非水毛细管电泳（NACE）方法，无需预处理即可同时测定马钱子及其制剂中的士的宁和马钱子碱。使用熔融石英毛细管柱（50 cm×75 μm内径）和在甲醇介质中含有30 mM醋酸铵、1.0%乙酸和15%乙腈（ACN）的运行缓冲液实现了最佳分离。施加电压为30.0 kV。通过在214 nm处的紫外检测分析物。研究了醋酸铵、乙酸和有机改性剂浓度对分析物电泳行为的影响。以槐定碱为内标建立的方法，士的宁和马钱子碱在5-1000 mg/mL范围内呈线性。马钱子及其制剂的提取物可直接进样测定，回收率在94.5%至104%之间。