Rudašová Marína, Masár Marián
Department of Analytical Chemistry, Faculty of Natural Sciences, Comenius University in Bratislava, Bratislava, Slovakia.
J Sep Sci. 2016 Jan;39(2):433-9. doi: 10.1002/jssc.201501025. Epub 2015 Nov 24.
A novel microchip electrophoresis method for the rapid and high-precision determination of N-acetylcysteine, a pharmaceutically active ingredient, in mucolytics has been developed. Isotachophoresis separations were carried out at pH 6.0 on a microchip with conductivity detection. The methods of external calibration and internal standard were used to evaluate the results. The internal standard method effectively eliminated variations in various working parameters, mainly run-to-run fluctuations of an injected volume. The repeatability and accuracy of N-acetylcysteine determination in all mucolytic preparations tested (Solmucol 90 and 200, and ACC Long 600) were more than satisfactory with the relative standard deviation and relative error values <0.7 and <1.9%, respectively. A recovery range of 99-101% of N-acetylcysteine in the analyzed pharmaceuticals predetermines the proposed method for accurate analysis as well. This work, in general, indicates analytical possibilities of microchip isotachophoresis for the quantitative analysis of simplified samples such as pharmaceuticals that contain the analyte(s) at relatively high concentrations.
已开发出一种新型微芯片电泳方法,用于快速、高精度地测定黏液溶解剂中药物活性成分N - 乙酰半胱氨酸。在pH 6.0条件下,于带有电导检测的微芯片上进行等速电泳分离。采用外标法和内标法评估结果。内标法有效消除了各种工作参数的变化,主要是进样体积的批间波动。在所测试的所有黏液溶解制剂(Solmucol 90和200以及ACC Long 600)中,N - 乙酰半胱氨酸测定的重复性和准确性都非常令人满意,相对标准偏差和相对误差值分别<0.7%和<1.9%。分析药物中N - 乙酰半胱氨酸的回收率范围为99 - 101%,这也预先确定了该方法可用于准确分析。总体而言,这项工作表明微芯片等速电泳在定量分析诸如含有相对高浓度分析物的药物等简化样品方面具有分析潜力。