Crego A L, Marina M L, Lavandera J L
Departamento de Química Analítica, Facultad de Química, Universidad de Alcalá, Alcalá de Henares (Madrid), Spain.
J Chromatogr A. 2001 May 11;917(1-2):337-45. doi: 10.1016/s0021-9673(01)00664-1.
Two simple, rapid, and efficient methods for the analysis of seven antifungal compounds have been developed by capillary zone electrophoresis. Resolutions higher than 1.5 were obtained using 0.025 M phosphate buffer (pH 2.30) (analysis time close to 9 min) or 0.2 M formic acid (pH 2.15) (analysis time close to 6 min), with an applied voltage of 20 kV and a temperature of 30 degrees C. The highest sensitivity and selectivity can be obtained using phosphate buffer but the shortest analysis times are achieved in the formic system. The analytical characteristics of the optimized methods were investigated. The reproducibility obtained for migration times (RSD(n = 10) < or = 1.0%) and peak areas (RSD(n = 10) < or = 4.3%) was acceptable, but better reproducibilities were obtained when verapamil was used as internal standard (RSD(n = 10) < 0.4% for relative migration times and RSD(n = 10) < or = 2.2% for peak area ratios). The lowest limit of detection was obtained for clotrimazole (0.12 microg/ml) and the highest for fluconazole and voriconazole (0.90 microg/ml). The lowest and the highest limits of quantitation were, respectively, 0.40 microg/ml for clotrimazole and 3.00 microg/ml for fluconazole and voriconazole.
通过毛细管区带电泳开发了两种简单、快速且高效的分析七种抗真菌化合物的方法。使用0.025 M磷酸盐缓冲液(pH 2.30)(分析时间接近9分钟)或0.2 M甲酸(pH 2.15)(分析时间接近6分钟),在20 kV的施加电压和30℃的温度下,分辨率高于1.5。使用磷酸盐缓冲液可获得最高的灵敏度和选择性,但在甲酸体系中可实现最短的分析时间。研究了优化方法的分析特性。迁移时间的重现性(RSD(n = 10) ≤ 1.0%)和峰面积的重现性(RSD(n = 10) ≤ 4.3%)是可以接受的,但当使用维拉帕米作为内标时,重现性更好(相对迁移时间的RSD(n = 10) < 0.4%,峰面积比的RSD(n = 10) ≤ 2.2%)。克霉唑的最低检测限为0.12微克/毫升,氟康唑和伏立康唑的最高检测限为0.90微克/毫升。克霉唑的最低定量限和最高定量限分别为0.40微克/毫升,氟康唑和伏立康唑的最高定量限为3.00微克/毫升。