流动注射-毛细管电泳法分离测定药物制剂中的四种活性成分

Separation and determination of four active components in medicinal preparations by flow injection-capillary electrophoresis.

作者信息

Liu Xiumei, Liu Lihong, Chen Hongli, Chen Xingguo

机构信息

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

出版信息

J Pharm Biomed Anal. 2007 Apr 11;43(5):1700-5. doi: 10.1016/j.jpba.2007.01.002. Epub 2007 Jan 8.

DOI:10.1016/j.jpba.2007.01.002

PMID:17337151

Abstract

A simple, rapid and accurate method for the separation and determination of paracetamol (Par), pseudoephedrine hydrochloride (Pse), dextromethorphan hydrobromide (Dex) and chlorphenamine hydrogen maleate (Chl) was developed by combination of flow injection and capillary zone electrophoresis for the first time. The analysis was carried out using an unmodified fused-silica capillary (75 mm x 75 microm i.d. x 375 microm o.d., effective separation length of 45 mm) and direct ultraviolet detection at 214 nm, 1.0 kV applied voltage. The optimized running buffer composed of 75 mM sodium borate-15% (v/v) acetonitrile (ACN) (pH* 9.30) was applied for the separation of the four analytes. The separation was achieved in 4.5 min. The sample throughput rate could reach up to 19 h(-1). The repeatability (defined as relative standard deviation) was 0.6%, 1.0%, 2.1%, 1.9% with peak height evaluation and 0.7%, 1.8%, 0.7%, 1.1% with peak area evaluation for Par, Pse, Dex and Chl, respectively. The limits of detection (S/N=3) were 0.22 microg/ml, 0.29 microg/ml, 0.42 microg/ml and 0.70 microg/ml for Par, Pse, Dex and Chl, respectively. The method was successfully applied to determine the four compounds in three cold medicines with recoveries in the range of 97.18-105.15%.

摘要

首次将流动注射与毛细管区带电泳相结合，开发出一种简单、快速且准确的方法，用于分离和测定对乙酰氨基酚（Par）、盐酸伪麻黄碱（Pse）、氢溴酸右美沙芬（Dex）和马来酸氯苯那敏（Chl）。分析采用未修饰的熔融石英毛细管（75 mm×75 μm内径×375 μm外径，有效分离长度45 mm），在214 nm处进行直接紫外检测，施加电压1.0 kV。优化后的运行缓冲液由75 mM硼酸钠 - 15%（v/v）乙腈（ACN）（pH* 9.30）组成，用于分离这四种分析物。分离在4.5分钟内完成。样品通量率可达19 h⁻¹。以峰高评估时，Par、Pse、Dex和Chl的重复性（定义为相对标准偏差）分别为0.6%、1.0%、2.1%、1.9%；以峰面积评估时，重复性分别为0.7%、1.8%、0.7%、1.1%。Par、Pse、Dex和Chl的检测限（S/N = 3）分别为0.22 μg/ml、0.29 μg/ml、0.42 μg/ml和0.70 μg/ml。该方法成功应用于测定三种感冒药中的这四种化合物，回收率在97.18 - 105.15%范围内。