Siluveru M, Stewart J T
Department of Medicinal Chemistry, College of Pharmacy, University of Georgia, Athens 30602-2352, USA.
J Chromatogr B Biomed Sci Appl. 1997 May 23;693(1):205-10. doi: 10.1016/s0378-4347(97)00017-0.
A capillary electrophoresis (CE) method for the quantification of R-(-)- and S-(+)-prilocaine in human serum was developed and validated. Stereoselective resolution was accomplished using 15 mM heptakis(2,6-di-methyl)-beta-cyclodextrin and 0.03 mM hexadecyltrimethylammonium bromide (HTAB) contained in 100 mM phosphate buffer, pH 2.5. Solid-phase extraction was used as a sample preparation technique to remove endogenous interferences. A 72-cm uncoated fused-silica capillary at a voltage of 25 kV and 30 degrees C was used for the analysis. The detection limits for R-(-)- and S-(+)-prilocaine were 38 ng/ml using 1 ml of human serum and the limits of quantitation were 45 ng/ml. The calibration curve was linear over the range of 45-750 ng/ml with procainamide as the internal standard. Precision and accuracy of the method were 2.86-8.50% and 3.29-7.40%, respectively, for R-(-)-prilocaine, and 3.94-9.17% and 2.0-6.73%, respectively, for S-(+)-prilocaine. The CE method was compared to an existing chiral HPLC method in terms of sensitivity and selectivity for the routine analysis of the drug.
建立并验证了一种用于定量测定人血清中R-(-)-和S-(+)-丙胺卡因的毛细管电泳(CE)方法。使用含有15 mM七(2,6-二甲基)-β-环糊精和0.03 mM十六烷基三甲基溴化铵(HTAB)的100 mM磷酸盐缓冲液(pH 2.5)实现立体选择性拆分。采用固相萃取作为样品制备技术以去除内源性干扰。分析使用一根72 cm未涂层熔融石英毛细管，电压为25 kV，温度为30℃。使用1 ml人血清时，R-(-)-和S-(+)-丙胺卡因的检测限为38 ng/ml，定量限为45 ng/ml。以普鲁卡因酰胺为内标，校准曲线在45-750 ng/ml范围内呈线性。该方法对R-(-)-丙胺卡因的精密度和准确度分别为2.86-8.50%和3.29-7.40%，对S-(+)-丙胺卡因的精密度和准确度分别为3.94-9.17%和2.0-6.73%。在该药物的常规分析中，将CE方法与现有的手性HPLC方法在灵敏度和选择性方面进行了比较。
