Al Azzam Khaldun M, Saad Bahruddin, Aboul-Enein Hassan Y
Universiti Sains Malaysia, Penang, Malaysia.
Biomed Chromatogr. 2010 Sep;24(9):977-81. doi: 10.1002/bmc.1395.
Capillary zone electrophoresis methods for the simultaneous determination of the beta-blocker drugs, atenolol, chlorthalidone and amiloride, in pharmaceutical formulations have been developed. The influences of several factors (buffer pH, concentration, applied voltage, capillary temperature and injection time) were studied. Using phenobarbital as internal standard, the analytes were all separated in less than 4 min. The separation was carried out in normal polarity mode at 25 degrees C, 25 kV and using hydrodynamic injection (10 s). The separation was effected in an uncoated fused-silica capillary (75 mum i.d. x 52 cm) and a background electrolyte of 25 mm H(3)PO(4) adjusted with 1 m NaOH solution (pH 9.0) and detection at 198 nm. The method was validated with respect to linearity, limit of detection and quantification, accuracy, precision and selectivity. Calibration curves were linear over the range 1-250 microg/mL for atenolol and chlorthalidone and from 2.5-250 microg/mL for amiloride. The relative standard deviations of intra- and inter-day migration times and corrected peak areas were less than 6.0%. The method showed good precision and accuracy and was successfully applied to the simultaneous determination of atenolol, chlorthalidone and amiloride in various pharmaceutical tablets formulations.
已开发出用于同时测定药物制剂中β受体阻滞剂药物阿替洛尔、氯噻酮和阿米洛利的毛细管区带电泳方法。研究了几个因素(缓冲液pH值、浓度、施加电压、毛细管温度和进样时间)的影响。以苯巴比妥为内标,所有分析物在不到4分钟内分离。分离在25℃、25 kV下以正常极性模式进行,采用流体动力学进样(10秒)。分离在未涂层熔融石英毛细管(内径75μm×52 cm)中进行,背景电解质为用1 m NaOH溶液调节至pH 9.0的25 mM H₃PO₄,并在198 nm处检测。该方法在线性、检测限和定量限、准确度、精密度和选择性方面进行了验证。阿替洛尔和氯噻酮的校准曲线在1-250μg/mL范围内呈线性,阿米洛利的校准曲线在2.5-250μg/mL范围内呈线性。日内和日间迁移时间以及校正峰面积的相对标准偏差小于6.0%。该方法具有良好的精密度和准确度,并成功应用于同时测定各种药物片剂制剂中的阿替洛尔、氯噻酮和阿米洛利。