Masár Marián, Hradski Jasna
Department of Analytical Chemistry, Faculty of Natural Sciences, Comenius University in Bratislava, Bratislava, Slovakia.
Methods Mol Biol. 2019;1906:99-111. doi: 10.1007/978-1-4939-8964-5_7.
Microchip isotachophoresis (μITP) is a miniaturized version of conventional isotachophoresis (ITP) characterized by low sample and buffer consumption and reduced waste production. μITP with universal conductivity detection is suitable for quantitative analysis of relatively simplified samples that contain analyte(s) at relatively high concentration, e.g., pharmaceutical preparations. Here we describe in detail a principle of μITP in terms of reaching highly precise results. A practical use of μITP is shown on the analyses of various pharmaceutical preparations for content of major constituents including active pharmaceutical ingredients as well as pharmaceutical counterions. The pharmaceuticals are treated only minimally prior to the ITP run on a microchip with coupled channels and sample injection channel with 0.9 μL volume. Developed method is suitable for rapid (analysis time up to 10 min), precise (less than 1% RSD of analyte zone length), and accurate (recovery of 98-101%) determination of major pharmaceutical ingredients using a method of internal standard for data evaluation.
微芯片等速电泳(μITP)是传统等速电泳(ITP)的微型化版本,其特点是样品和缓冲液消耗低,废物产生减少。具有通用电导检测功能的μITP适用于对含有相对高浓度分析物的相对简单样品进行定量分析,例如药物制剂。在此,我们详细描述了μITP在获得高精度结果方面的原理。μITP在分析各种药物制剂中的主要成分(包括活性药物成分以及药物抗衡离子)含量方面的实际应用得到了展示。在具有耦合通道和0.9 μL体积的样品注入通道的微芯片上进行ITP运行之前,对药物的处理非常少。所开发的方法适用于使用内标法进行数据评估,快速(分析时间长达10分钟)、精确(分析物区带长度的相对标准偏差小于1%)且准确(回收率为98 - 101%)地测定主要药物成分。