Vargas G, Havel J, Hadasová E
Department of Analytical Chemistry, Faculty of Science, Masaryk University, Brno, Czech Republic.
J Chromatogr A. 1997 Jun 6;772(1-2):271-6. doi: 10.1016/s0021-9673(97)00106-4.
In this work a new sensitive capillary zone electrophoresis method for the direct determination of procainamide (PA) and N-acetylprocainamide (NAPA) in pharmaceutical formulations and urine samples without any extraction and/or preconcentration steps has been developed. The determination was carried out in a fused-silica capillary of 43.5 cm (35.9 cm length to the detector) x 0.75 micron J.D. Phosphate 0.05 M buffer was used as the background electrolyte and 10 kV separation voltage was applied. The separation of PA and NAPA is possible in a wide range of pH from 1.7 to 9.7. However, in order to avoid the effect of the urine matrix, it is optimal to work at pH 7.7. The determination of PA and NAPA takes less than 5 min while high resolution is achieved. The detection limits obtained, 1.235 micrograms/ml and 0.359 microgram/ml for PA and NAPA respectively, are lower than those for GC method normally reported.
在本研究中,开发了一种新型灵敏的毛细管区带电泳方法,用于直接测定药物制剂和尿液样本中的普鲁卡因胺(PA)和N-乙酰普鲁卡因胺(NAPA),无需任何萃取和/或预浓缩步骤。测定在一根43.5 cm(至检测器的长度为35.9 cm)×0.75微米内径的熔融石英毛细管中进行。使用0.05 M磷酸盐缓冲液作为背景电解质,并施加10 kV的分离电压。在1.7至9.7的宽pH范围内可以实现PA和NAPA的分离。然而,为了避免尿液基质的影响,最佳工作pH值为7.7。PA和NAPA的测定耗时不到5分钟,同时实现了高分辨率。获得的检测限分别为PA 1.235微克/毫升和NAPA 0.359微克/毫升,低于通常报道的气相色谱法的检测限。