Department of Chemistry, Xixi Campus, Zhejiang University, Hangzhou 310028, China.
Talanta. 2011 Jul 15;85(1):123-9. doi: 10.1016/j.talanta.2011.03.037. Epub 2011 Mar 30.
The development of a reversed phase liquid chromatographic method for the simultaneous determination of seven angiotensin converting enzyme (ACE) inhibitors; five drugs namely benazepril HCl (BZL), enalapril maleate (ENL), fosinopril sodium (FSP), lisinopril (LSP) and ramipril (RMP) and two metabolites captopril disulfide (CPD) and enalaprilat (ENT) together with hydrochlorothiazide (HCT) is described. The method can serve as a substitute for many published papers for the analysis of the targeted compounds with or without hydrochloothiazide in pharmaceutical formulations as well as in spiked human plasma and urine samples. The method utilizes a simple gradient procedure for the separation in a 11 min run time using acetonitrile aqueous ammonia buffer (pH 9) solution and an Extend RP-C18 (25 μm particle size, 4.6 mm×250 mm, Agilent) HPLC column. The effluent was monitored on a UV detector at 215 nm. The effect of pH, solvent strength and analysis time on the peak shape and quantification were carefully studied in order to optimize the method. Adopting the proposed procedure, the analytes produce well-shaped peaks with good linear relationship over the investigated concentration ranges. The limits of detection (LOD) and limits of quantification (LOQ) from standard drug solutions lie in the range of 17-64 and 56-212 ng mL(-1), respectively. Correlation coefficient values (r) higher than 0.997 were obtained for all the studied drugs in spiked human plasma and urine samples. The intra-day and inter-day precision of the method was evaluated with relative standard deviation values being satisfactory for their purposed analysis. The method was validated with respect to specificity, recovery, accuracy, precision and linearity.
描述了一种反相液相色谱法同时测定七种血管紧张素转化酶（ACE）抑制剂的方法；五种药物分别为盐酸贝那普利（BZL）、马来酸依那普利（ENL）、福辛普利钠（FSP）、赖诺普利（LSP）和雷米普利（RMP）以及两种代谢物卡托普利二硫化物（CPD）和依那普利拉（ENT）以及氢氯噻嗪（HCT）。该方法可替代许多已发表的论文，用于分析药物制剂中是否含有氢氯噻嗪的目标化合物，以及加标人血浆和尿液样品。该方法在 11 分钟的运行时间内使用乙腈-氨水缓冲液（pH9）溶液和 Extend RP-C18（25μm 粒径，4.6mm×250mm，Agilent）HPLC 柱进行简单的梯度分离。在 215nm 处用紫外检测器监测流出物。为了优化方法，仔细研究了 pH、溶剂强度和分析时间对峰形和定量的影响。采用所提出的程序，分析物在考察的浓度范围内产生良好形状的峰，具有良好的线性关系。从标准药物溶液中获得的检测限（LOD）和定量限（LOQ）分别在 17-64 和 56-212ngmL-1范围内。在加标人血浆和尿液样品中，所有研究药物的相关系数（r）均高于 0.997。该方法的日内和日间精密度用相对标准偏差值进行评估，对于其目的分析是令人满意的。该方法在特异性、回收率、准确性、精密度和线性方面均经过验证。
