Özdemir Filiz Arıöz, Akyüz Atalay
Faculty of Pharmacy, Department of Analytical Chemistry, University of Marmara, 34688, Usküdar, Istanbul, Turkey
Faculty of Pharmacy, Department of Analytical Chemistry, University of Marmara, 34688, Usküdar, Istanbul, Turkey.
J Chromatogr Sci. 2014 Aug;52(7):685-90. doi: 10.1093/chromsci/bmt099. Epub 2013 Jul 9.
A new, simple, rapid and specific reversed-phase high-performance liquid chromatography (HPLC) method was developed and validated for the simultaneous determination of amlodipine besylate and aliskiren hemifumarate. The HPLC separation was achieved on an RP-18 column (250 × 4.6 mm) using a mobile phase of triethylamine-orthophosphoric acid buffer (50 mM, pH 3.0), acetonitrile and methanol (50:40:10, v/v/v) at a flow rate of 1 mL/min. The method was validated for specificity, linearity, precision, accuracy and robustness. The degree of linearity of the calibration curves, the percent recovery values of amlodipine and aliskiren and the limits of detection (LOD) and quantification (LOQ) for the HPLC method were determined. The linearity of the method was found to be in the concentration range of 5.0-50.0 µg/mL for aliskiren hemifumarate and 2.65-26.50 µg/mL for amlodipine besylate, LOD and LOQ values were 0.51, 0.95, 1.70 and 3.18 µg/mL for amlodipine besylate and aliskiren hemifumarate. The proposed method was successfully applied to amlodipine besylate and aliskiren hemifumarate in pharmaceutical dosage mixtures without any interference from the excipients. The method was found to be precise, accurate, reproducible and robust. The results agreed with those obtained using the developed reference method.
建立并验证了一种新的、简单、快速且特异的反相高效液相色谱（HPLC）法，用于同时测定苯磺酸氨氯地平和阿利吉仑半富马酸盐。HPLC分离在RP - 18柱（250×4.6 mm）上进行，流动相为三乙胺 - 正磷酸缓冲液（50 mM，pH 3.0）、乙腈和甲醇（50:40:10，v/v/v），流速为1 mL/min。该方法在特异性、线性、精密度、准确度和稳健性方面得到了验证。测定了校准曲线的线性程度、氨氯地平和阿利吉仑的回收率百分比值以及HPLC法的检测限（LOD）和定量限（LOQ）。该方法的线性范围为阿利吉仑半富马酸盐5.0 - 50.0 μg/mL，苯磺酸氨氯地平2.65 - 26.50 μg/mL，苯磺酸氨氯地平和阿利吉仑半富马酸盐的LOD和LOQ值分别为0.51、0.95、1.70和3.18 μg/mL。所提出的方法成功应用于药物剂型混合物中的苯磺酸氨氯地平和阿利吉仑半富马酸盐，无任何辅料干扰。该方法被发现是精确、准确、可重现且稳健的。结果与使用所开发的参考方法获得的结果一致。
