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高效液相色谱法转移研究同时测定七种血管紧张素 II 受体阻滞剂。

HPLC method transfer study for simultaneous determination of seven angiotensin II receptor blockers.

机构信息

Ministry of Health, Directorate of Health Affairs, Ismailia Health Administration, Ismailia, Egypt.

Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Suez Canal University, Ismailia, Egypt.

出版信息

J Sep Sci. 2020 Apr;43(8):1398-1405. doi: 10.1002/jssc.201900534. Epub 2020 Feb 16.

Abstract

In this study, a sensitive high-performance liquid chromatography method was developed and validated for the simultaneous determination of seven angiotensin II receptor blockers, namely, hydrochlorothiazide, chlorthalidone, eprosartan mesylate, valsartan, losartan potassium, irbesartan, and candesartan cilexetil. Different chromatographic parameters were tested and fully optimized. Best chromatographic separation was accomplished on a reversed-phase octadecylsilyl column (250 × 4.6 mm id; 5 μm) under gradient elution using methanol/sodium phosphate monobasic buffer (0.01 M, pH 6.5) as mobile phase. The detection of target analytes was obtained at 254 nm. The pH of the buffer has been selected according to Marvin sketch software. The proposed method was validated according to ICH guidelines and showed good precision (relative standard deviation < 1), good linearity (square of correlation coefficient ≥ 0.999), and high accuracy (between 98 and 102%) with detection limit and quantitation limit (40 and 160 ng/mL, respectively) for all the detected analytes.

摘要

在这项研究中,开发并验证了一种灵敏的高效液相色谱法,用于同时测定七种血管紧张素 II 受体阻滞剂,即氢氯噻嗪、氯噻酮、甲磺酸依普罗沙坦、缬沙坦、氯沙坦钾、厄贝沙坦和坎地沙坦西酯。测试并充分优化了不同的色谱参数。在反相十八烷基硅烷柱(250×4.6mm id;5μm)上,以梯度洗脱的方式,使用甲醇/磷酸单碱基缓冲液(0.01M,pH 6.5)作为流动相,实现了最佳的色谱分离。目标分析物的检测在 254nm 处获得。缓冲液的 pH 值是根据 Marvin sketch 软件选择的。该方法按照 ICH 指南进行了验证,具有良好的精密度(相对标准偏差<1%)、良好的线性(相关系数平方≥0.999)和高准确度(检测限和定量限分别为 40 和 160ng/mL),所有检测到的分析物均具有良好的准确度(98%至 102%之间)。

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