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目的:建立高效液相色谱-质谱法测定人血浆中单硝酸异山梨酯浓度的方法。方法:以茶碱为内标,血浆样品经乙酸乙酯提取后,用Zorbax XDB-C_(18)分析柱(150 mm×2.1 mm,5μm),流动相为A:0.01%冰乙酸,流速为0.15 ml·min~(-1);B:甲醇,流速为0.05 ml·min~(-1)。采用四极杆质谱检测器大气压电喷雾离子源。负离子检测,检测离子:单硝酸异山梨酯为m/z 250,内标为m/z 179。结果:血浆中单硝酸异山梨酯浓度在0.0125～1.2 mg·L~(-1)范围内线性关系良好(r=0.999 6),最低检测浓度为0.0125 mg·L~(-1)。平均提取回收率为86.0%,日内RSD<8.9%。日间RSD<4.8%。结论:该法简便、快速,灵敏度高,可用于单硝酸异山梨酯制剂的药动学研究。
Objective: To establish a method for the determination of isosorbide mononitrate in human plasma by high performance liquid chromatography-mass spectrometry. Methods: Theophylline was used as an internal standard. The plasma samples were extracted with ethyl acetate. The mobile phase consisted of A: 0.01% glacial acetic acid and the mobile phase was Zorbax XDB-C 18 column (150 mm × 2.1 mm, 0.15 ml · min -1; B: methanol at a flow rate of 0.05 ml · min -1. A quadrupole mass spectrometer was used for atmospheric pressure electrospray ionization. Negative ion detection, detection of ions: Isosorbide mononitrate m / z 250, internal standard m / z 179. RESULTS: The concentration of isosorbide mononitrate in plasma ranged from 0.0125 to 1.2 mg · L ~ (-1) with good linearity (r = 0.999 6) and the lowest concentration was 0.0125 mg · L -1. The average extraction recovery rate was 86.0%, RSD <8.9%. Day RSD <4.8%. Conclusion: The method is simple, rapid, sensitive and can be applied to the pharmacokinetics of isosorbide mononitrate preparations.