Qin Feng, Wang Dan, Yang Shuyan, Jing Lijuan, Xiong Zhili, Li Famei
Department of Analytical Chemistry, Shenyang Pharmaceutical University, Shenyang 110016, People's Republic of China.
Biomed Chromatogr. 2012 Jun;26(6):691-6. doi: 10.1002/bmc.1715. Epub 2011 Sep 19.
A rapid, selective and sensitive high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed to determine lisinopril in human plasma. Sample pretreatment involved a one-step protein precipitation with methanol of 0.1 mL plasma. Analysis was performed on an Inertsil ODS-3 column (2.1 × 50 mm i.d., 3 µm) with mobile phase consisting of methanol-water (containing 0.2% formic acid; 55:45, v/v). The detection was performed on a triple quadrupole tandem mass spectrometer in multiple reaction monitoring mode via an electrospray ionization source. Each plasma sample was chromatographed within 2.5 min. The linear calibration curves for lisinopril were obtained in the concentration range of 1.03-206 ng/mL (r(2) ≥ 0.99) with a lower limit of quantification of 1.03 ng/mL. The intra- and inter-day precisions (relative standard deviation) were not higher than 11%, and accuracy (relative error) was within ±6.8%, determined from quality control samples for lisinopril, which corresponded to the guidance of the Food and Drug Administration. The method described herein was fully validated and successfully applied to the pharmacokinetic study of lisinopril tablets in healthy male volunteers after oral administration.
建立了一种快速、选择性和灵敏的高效液相色谱-串联质谱（HPLC-MS/MS）法测定人血浆中的赖诺普利。样品预处理包括用0.1 mL甲醇对血浆进行一步蛋白沉淀。分析在Inertsil ODS-3柱（内径2.1×50 mm，3 µm）上进行，流动相由甲醇-水（含0.2%甲酸；55:45，v/v）组成。检测在三重四极杆串联质谱仪上通过电喷雾电离源在多反应监测模式下进行。每个血浆样品在2.5分钟内完成色谱分析。赖诺普利的线性校准曲线在1.03-206 ng/mL浓度范围内获得（r(2)≥0.99），定量下限为1.03 ng/mL。日内和日间精密度（相对标准偏差）不高于11%，准确度（相对误差）在±6.8%以内，由赖诺普利的质量控制样品确定，符合美国食品药品监督管理局的指导原则。本文所述方法经过充分验证，并成功应用于健康男性志愿者口服赖诺普利片后的药代动力学研究。
