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利用实验设计开发一种用于定量卡托普利的毛细管区带电泳方法。

The use of experimental design for the development of a capillary zone electrophoresis method for the quantitation of captopril.

作者信息

Mukozhiwa S Y, Khamanga S M M, Walker R B

出版信息

Pharmazie. 2017 Sep 1;72(9):518-524. doi: 10.1691/ph.2017.7071.

Abstract

A capillary zone electrophoresis (CZE) method for the quantitation of captopril (CPT) using UV detection was developed. Influence of electrolyte concentration and system variables on electrophoretic separation was evaluated and a central composite design (CCD) was used to optimize the method. Variables investigated were pH, molarity, applied voltage and capillary length. The influence of sodium metabisulphite on the stability of test solutions was also investigated. The use of sodium metabisulphite prevented degradation of CPT over 24 hours. A fused uncoated silica capillary of 67.5cm total and 57.5 cm effective length was used for analysis. The applied voltage and capillary length affected the migration time of CPT significantly. A 20 mM phosphate buffer adjusted to pH 7.0 was used as running buffer and an applied voltage of 23.90 kV was suitable to effect a separation. The optimized electrophoretic conditions produced sharp, well-resolved peaks for CPT and sodium metabisulphite. Linear regression analysis of the response for CPT standards revealed the method was linear (R2 = 0.9995) over the range 5-70 μg/mL. The limits of quantitation and detection were 5 and 1.5 μg/mL. A simple, rapid and reliable CZE method has been developed and successfully applied to the analysis of commercially available CPT products.

摘要

建立了一种采用紫外检测定量卡托普利(CPT)的毛细管区带电泳(CZE)方法。评估了电解质浓度和系统变量对电泳分离的影响,并采用中心复合设计(CCD)对该方法进行优化。所研究的变量包括pH值、摩尔浓度、施加电压和毛细管长度。还研究了焦亚硫酸钠对测试溶液稳定性的影响。使用焦亚硫酸钠可防止CPT在24小时内降解。采用总长度为67.5cm、有效长度为57.5cm的熔融未涂层石英毛细管进行分析。施加电压和毛细管长度对CPT的迁移时间有显著影响。使用pH值调至7.0的20 mM磷酸盐缓冲液作为运行缓冲液,施加23.90 kV的电压适合实现分离。优化后的电泳条件为CPT和焦亚硫酸钠产生了尖锐、分离良好的峰。CPT标准品响应的线性回归分析表明,该方法在浓度范围为5 - 70μg/mL时呈线性(R2 = 0.9995)。定量限和检测限分别为5μg/mL和1.5μg/mL。已开发出一种简单、快速且可靠的CZE方法,并成功应用于市售CPT产品的分析。

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