Alanazi Amer M, Abdelhameed Ali S, Khalil Nasr Y, Khan Azmat A, Darwish Ibrahim A
Acta Pharm. 2014 Jun;64(2):187-98. doi: 10.2478/acph-2014-0014.
A simple, sensitive and accurate HPLC method with high throughput has been developed and validated for the simultaneous determination of irbesartan (IRB) and hydrochlorothiazide (HCT) in combined pharmaceutical dosage forms. The proposed method employed, for the first time, a monolithic column in the analysis. Optimal chromatographic separation of the analytes was achieved on Chromolith(®) Performance RP-18e column using a mobile phase consisting of phosphate buffer (pH 4)/acetonitrile (50:50, V/V) pumped isocratically at a flow rate of 1.0 mL min(-1). The eluted analytes were monitored with a UV detector set at 270 nm. Under the optimum chromatographic conditions, linear relationship with a good correlation coefficient (R ≥ 0.9997) was found between the peak area and the corresponding concentrations of both IRB and HCT in the ranges of 10-200 and 1-20 ng mL(-1). The limits of detection were 2.34 and 0.03 ng mL(-1) for IRB and HCT, respectively. The intra- and inter-assay precisions were satisfactory as the RSD values did not exceed 3 %. The accuracy of the proposed method was > 97 %. The proposed method had high throughput as the analysis involved a simple procedure and a very short run-time of < 3 min. The results demonstrated that the method is applicable in the quality control of combined pharmaceutical tablets containing IRB and HCT.
已开发并验证了一种简单、灵敏、准确且高通量的高效液相色谱法，用于同时测定复方药物剂型中的厄贝沙坦（IRB）和氢氯噻嗪（HCT）。所提出的方法首次在分析中采用了整体柱。使用由磷酸盐缓冲液（pH 4）/乙腈（50:50，V/V）组成的流动相，以1.0 mL min⁻¹的流速等度泵入，在Chromolith(®) Performance RP - 18e柱上实现了分析物的最佳色谱分离。用设置在270 nm的紫外检测器监测洗脱的分析物。在最佳色谱条件下，IRB和HCT的峰面积与相应浓度在10 - 200和1 - 20 ng mL⁻¹范围内呈良好的线性关系，相关系数（R≥0.9997）。IRB和HCT的检测限分别为2.34和0.03 ng mL⁻¹。批内和批间精密度令人满意，相对标准偏差（RSD）值不超过3%。所提出方法的准确度>97%。由于该分析涉及简单的程序且运行时间非常短，<3分钟，所以所提出的方法具有高通量。结果表明该方法适用于含IRB和HCT的复方药片片剂的质量控制。
