Salim Mohamed M, Ebeid Walid M, El-Enany Nahed, Belal Fathalla, Walash Mohamed, Patonay Gabor
Department of Chemistry, Georgia State University, Atlanta, GA, USA; Department of Analytical Chemistry, Faculty of Pharmacy, University of Mansoura, Mansoura, Egypt.
J Sep Sci. 2014 May;37(9-10):1206-13. doi: 10.1002/jssc.201301140. Epub 2014 Mar 25.
A novel, specific, reliable, and accurate capillary zone electrophoretic method was developed and validated for the simultaneous determination of aliskiren hemifumarate, amlodipine besylate, and hydrochlorothiazide in their triple mixture dosage form. Separation was carried out in a fused-silica capillary (57.0 cm total length and 50.0 cm effective length, 75.6 μm internal diameter) by applying a potential of 17 kV and a running buffer consisting of 40 mM phosphate buffer at pH 6.0 with UV detection at 245 nm. The method was suitably validated with respect to specificity, linearity, LOD, and LOQ, accuracy, precision, and robustness. The method showed good linearity in the ranges 1-10, 2.5-25, and 30-300 μg/mL with LODs of 0.11, 0.33, and 5.83 μg/mL for amlodipine besylate, hydrochlorothiazide, and aliskiren hemifumarate, respectively. The proposed method was successfully applied for the analysis of the studied drugs in their coformulated tablets. The results of the proposed method were statistically compared with those obtained by the RP-HPLC reference method revealing no significant differences in the performance of the methods regarding accuracy and precision.
开发并验证了一种新颖、特异、可靠且准确的毛细管区带电泳方法，用于同时测定半富马酸阿利吉仑、苯磺酸氨氯地平和氢氯噻嗪三联混合剂型中的这些成分。在熔融石英毛细管（总长57.0 cm，有效长度50.0 cm，内径75.6 μm）中进行分离，施加17 kV的电压，运行缓冲液为pH 6.0的40 mM磷酸盐缓冲液，在245 nm处进行紫外检测。该方法在特异性、线性、检测限、定量限、准确度、精密度和稳健性方面得到了适当验证。该方法在1 - 10、2.5 - 25和30 - 300 μg/mL范围内显示出良好的线性，苯磺酸氨氯地平、氢氯噻嗪和半富马酸阿利吉仑的检测限分别为0.11、0.33和5.83 μg/mL。所提出的方法成功应用于对其复方片剂中所研究药物的分析。将所提出方法的结果与反相高效液相色谱参考方法获得的结果进行统计学比较，结果表明在准确度和精密度方面，两种方法的性能无显著差异。
