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目的:建立测定大鼠血浆中咪哒唑仑浓度的液相色谱串联质谱法。方法:以伊曲康唑为内标,色谱柱为XTerra MSC18(150mm×2.1mm,3.5μm);流动相为乙腈-0.02%醋酸铵(75∶25);流速为0.2mL.min-1;质谱仪为电喷雾-三重四极杆质谱,以多反应监测(MRM)方式对咪哒唑仑(m/z326.2→m/z291.2)和伊曲康唑(m/z705.3→m/z392.1)进行测定。结果:咪哒唑仑在125～50 000μg.L-1范围内线性关系良好(r=0.996 8),最低检测限为5.0μg.L-1。低、中、高浓度的平均回收率为97.22%,101.88%,90.57%;日内及日间精密度均小于10%。结论:本方法简单、快速、灵敏,能有效检测大鼠血浆中咪哒唑仑的浓度。
Objective: To establish a liquid chromatography-tandem mass spectrometry method for the determination of midazolam in rat plasma. Methods: Itraconazole was used as internal standard. The column was XTerra MSC18 (150mm × 2.1mm, 3.5μm). The mobile phase was acetonitrile-0.02% ammonium acetate (75:25), the flow rate was 0.2mL.min-1. The mass spectrometer was electrospray-triple quadrupole mass spectrometry (MS-MS / MS), and multivariate MRM (m / z 326.2 → m / z 291.2) and itraconazole (m / z 705.3 → m / z 392.1). RESULTS: Midazolam had a good linearity (r = 0.996 8) in the range of 125 to 50 000 μg.L-1 with a minimum detectable limit of 5.0 μg.L-1. The average recoveries of low, medium and high concentrations were 97.22%, 101.88% and 90.57%, respectively. The intra- and inter-day precision were less than 10%. Conclusion: The method is simple, rapid and sensitive and can effectively detect the concentration of midazolam in rat plasma.