HPLC-MS法测定人血浆中厄贝沙坦的浓度

目的建立快速、灵敏的HPLC-MS法测定人血浆中厄贝沙坦的浓度，并研究厄贝沙坦片在健康人体内的药动学。方法以对乙酰氨基酚为内标，血浆样品经乙酸乙酯萃取后，以乙腈-水（40：60，v／v）为流动相，经Sinochrom ODS-BP C18柱分离，以负离子方式检测，扫描方式为选择离子监测（SIM）。用于定量分析的离子分别为m／z 427．35（厄贝沙坦）和m／z 150．10（对乙酰氨基酚）。结果测定血浆中厄贝沙坦方法的线性范围为20～5000ng·mL^-1（r〉0．997），定量下限20ng·mL^-1。日内RSD％为3．8％～6．1％，日间RSD％为3．3％～14．4％，厄贝沙坦提取回收率为71．3％～87．9％；内标对乙酰氨基酚提取回收率为93．7％。每个样品分析时间为4．0min。应用此法研究了20名健康受试者单剂量口服150mg厄贝沙坦片后的药动学特点。结论该法选择性强，灵敏度高，适用于厄贝沙坦的临床药动学研究。

Determination of irbesartan in human plasma by HPLC-MS

Objective To develop a fast and sensitive HPLC-MS method for the determination of irbesartan concentration in human plasma and study the pharmacokinetics in healthy volunteers. Methods Plasma was treated by a simple extraction using ethyl acetate, and then separated on Sinochrom ODS-BPC18 column with a mobile phase of acetonitrile-water （40 ： 60, v/v）. Acetaminophen was used as the internal standard. Irbesartan was determined by HPLC-ESI/ MS in selected ion monitoring （SIM） in negative ion mode, m/z 427.35 and rn/z 150.10 were used to qualify irbesartan and acetaminophen, respectively. Results The linear calibration curve was obtained at 20--5 000 ng·mL^-1 （r〉 0. 997）. The lower limit of quantification was 20 ng ·mL^-1. The inter-day precision （RSD） was 3.8%--6.1%, and the intra-day precision （RSD） was 3.3%0--14.4%. The recovery for irbesatan was 72.3%--87.9%. The recovery for internal standard was 97.3%. The total chromatographic running time was 4.0 rain. The method was used in a pharmacokinetic study in 20 healthy volunteers after a single oral dose of 150 mg irbesartan. Conclusion The method is selective, sensitive, and suitable for the clinical investigation of irbesartan pharmacokinetics.