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用于测定人血浆中坎地沙坦的高效液相色谱法的建立与验证

Development and validation of HPLC method for the determination of Candesartan in human plasma.

作者信息

Hamid Shaista, Beg Anwar Ejaz, Muhammad Iyad Naeem, Hassan Sohail, Hassan Amir, Akram Arfa, Alladin Neyama

机构信息

Department of Pharmaceutics, Faculty of Pharmacy and Pharmaceutical Sciences, University of Karachi, Karachi, Pakistan.

Department of Pharmaceutics, Faculty of Pharmacy, Ziauddin University, Karachi, Pakistan.

出版信息

Pak J Pharm Sci. 2018 Nov;31(6):2323-2327.

PMID:30473499
Abstract

Candesartan (CAN), an ARB-blocker, antihypertensive, was analyzed in human plasma by a simple, accurate and precise RP-HPLC (reverse phase-High performance liquid chromatography assay method which was then validated for its accuracy, specificity and precision. The mobile phase has a constitution of acetone, diethylamine and distilled water, while Phosphoric acid was used to adjust the pH to 2.5±0.1. This mobile phase was run at 1.1ml/min and the fluorescence wavelength was set to 392 nm. A C-18 HPLC, column particle size (5 μm) Mediterranean Sea ® L x 1.D. 25cm x 4.6 mm (Supelcosil) , with auto sampler injection volume of 30μl ,an internal standard Valsartan was utilized for chromatographic detection. Candesartan took a retention time of 6±0.5 minutes. This method was validated by the parameters of selectivity, accuracy, precision, repeatability, reproducibility, recovery, linearity and stability. Candesartan's calibration curves were found to be linear in the range of 200ng/ml to 3.125ng/ml and the coefficient of determination (r) was found to be 0.99. Analytical recovery obtained was above 88%. Hence, this method has been found to be useful for determining Candesartan in plasma.

摘要

坎地沙坦(CAN)是一种血管紧张素Ⅱ受体拮抗剂类降压药,采用简单、准确且精密的反相高效液相色谱法(RP-HPLC)对其在人体血浆中的含量进行分析,随后对该方法的准确性、特异性和精密度进行了验证。流动相由丙酮、二乙胺和蒸馏水组成,用磷酸将pH值调至2.5±0.1。该流动相以1.1ml/分钟的流速运行,荧光波长设定为392nm。使用粒径为5μm的C-18高效液相色谱柱(地中海海®L x 内径25cm x 4.6mm,Supelcosil公司生产),自动进样器进样体积为30μl,以内标物缬沙坦进行色谱检测。坎地沙坦的保留时间为6±0.5分钟。通过选择性、准确性、精密度、重复性、重现性、回收率、线性和稳定性等参数对该方法进行了验证。发现坎地沙坦的校准曲线在200ng/ml至3.125ng/ml范围内呈线性,测定系数(r)为0.99。获得的分析回收率高于88%。因此,已发现该方法可用于测定血浆中的坎地沙坦。

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