Valese Andressa C, Spudeit Daniel A, Dolzan Maressa D, Bretanha Lizandra C, Vitali Luciano, Micke Gustavo A
Department of Food Science Technologies, Federal University of Santa Catarina, Florianopolis, SC, Brazil.
Departamento de Química, CFM, UFSC, Campus Universitário, Trindade, CP 476, 88040-900 Florianópolis, SC, Brazil.
J Anal Methods Chem. 2016;2016:4126810. doi: 10.1155/2016/4126810. Epub 2016 Mar 16.
This paper reports the development of a subminute separation method by capillary zone electrophoresis in an uncoated capillary using multiple injection procedure for the determination of lidocaine in samples of pharmaceutical formulations. The separation was performed in less than a minute leading to doing four injections in a single run. The cathodic electroosmotic flow contributed to reducing the analyses time. The background electrolyte was composed of 20 mmol L(-1) 2-amino-2-(hydroxymethyl)-1,3-propanediol and 40 mmol L(-1) 2-(N-morpholino)ethanesulfonic acid at pH 6.1. The internal standard used was benzylamine. Separations were performed in a fused uncoated silica capillary (32 cm total length, 23.5 cm effective length, and 50 μm internal diameter) with direct UV detection at 200 nm. Samples and standards were injected hydrodynamically using 40 mbar/3 s interspersed with spacer electrolyte using 40 mbar/7 s. The electrophoretic system was operated under constant voltage of 30 kV with positive polarity on the injection side. The evaluation of some analytical parameters of the method showed good linearity (r (2) > 0.999), a limit of detection 0.92 mg L(-1), intermediate precision better than 3.2% (peak area), and recovery in the range of 92-102%.
本文报道了一种在未涂层毛细管中采用多次进样程序的毛细管区带电泳亚分钟分离方法的开发,用于测定药物制剂样品中的利多卡因。分离在不到一分钟内完成,单次运行可进行四次进样。阴极电渗流有助于缩短分析时间。背景电解质由pH 6.1的20 mmol L⁻¹ 2-氨基-2-(羟甲基)-1,3-丙二醇和40 mmol L⁻¹ 2-(N-吗啉代)乙磺酸组成。使用的内标为苄胺。在总长度32 cm、有效长度23.5 cm、内径50 μm的熔融未涂层石英毛细管中进行分离,采用200 nm的直接紫外检测。样品和标准品通过40 mbar/3 s的流体动力学进样,间隔使用40 mbar/7 s的间隔电解质。电泳系统在30 kV的恒定电压下运行,进样侧为正极性。该方法一些分析参数的评估显示出良好的线性(r² > 0.999)、检测限为0.92 mg L⁻¹、中间精密度优于3.2%(峰面积),回收率在92 - 102%范围内。