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目的建立测定人血浆中艾司西酞普兰浓度的高效液相色谱-质谱-质谱联用法。方法血浆样品经甲醇沉淀后进行分析。色谱柱Lichrospher CN柱150 mm×4 .6 mmI .D.5μm,流动相甲醇∶水(含15 mmol·L-1乙酸铵)∶甲酸(72∶28∶0 .1 ,v/v/v) ,流速1 .0 ml·min-1,电喷雾离子化三重四极杆串联质谱检测,以选择离子反应监测(SRM)扫描方式进行检测,采用选择离子反应监测(SRM)方式进行定量分析,用于监测的离子为m/z325 .0→234 .0(西酞普兰)和m/z409 .1→238 .1(氨氯地平,内标)。结果线性范围为0 .20 ~50 .00 ng·ml-1,最低定量浓度为0 .20 ng·ml-1,应用此法测试了10名健康受试者口服草酸艾司西酞普兰片(10 mg)后不同时间的血药浓度,得到艾司西酞普兰药动学参数,Cmax为9 .21±2 .10 ng·ml-1,Tmax为3 .75 ±1 .04 h ,AUC0 -t为514 .6 ± 152 .3 ng·h·ml-1,AUC0 -∞为540 .5 ±162 .3 ng·h·ml-1,t1/2为34 .06 ±7 .71 h及Ke为0 .021±0 .004 h-1。结论该法专属、灵敏、简便、快速,适用于人血浆中艾司西酞普兰浓度的测定。
Objective To establish a method for the determination of escitalopram in human plasma by high performance liquid chromatography-mass spectrometry-mass spectrometry. Methods Plasma samples were analyzed by methanol precipitation. Column Lichrospher CN 150 mm × 4.6 mmI .D.5 μm, mobile phase methanol: water (containing 15 mmol·L -1 ammonium acetate): formic acid (72:28:0.1, v / v / v) , Flow rate of 1.0 ml · min-1, electrospray ionization triple quadrupole tandem mass spectrometry, selective ion monitoring (SRM) The ions monitored were m / z 325.0 -> 234.0 (citalopram) and m / z 409.1 -> 238.1 (amlodipine, internal standard). Results The linear range was from 0.20 to 50.00 ng · ml-1 and the lowest concentration was 0.20 ng · ml-1. Ten healthy volunteers were enrolled in this study. Escitalopram oxalate 10 mg), the pharmacokinetic parameters of Escitalopram were obtained. The Cmax was 9.21 ± 2.10 ng · ml-1, the Tmax was 3.75 ± 1.04 h, the AUC0- t was 514.6 ± 152.3 ng · h · ml-1, AUC0 -∞ was 540.5 ± 162.3 ng · h · ml-1, t1 / 2 was 34.06 ± 7.71 h and Ke Was 0. 021 ± 0 .004 h-1. Conclusion This method is sensitive, simple and rapid and is suitable for the determination of escitalopram concentration in human plasma.