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目的建立测定人血浆中齐拉西酮浓度的反相高效液相串联质谱电喷雾检测法(LC-ESI-MS/MS)。方法以迪马公司C18反相柱(Dialmonsil C18 column,4.6 mm×150 mm,5μm)为色谱柱,流动相为甲醇-5 mmol.L-1甲酸铵(90∶10),流速为1 mL.min-1,柱温:25℃,以醋酸乙酯-二氯甲烷(4∶1)为提取剂。样品经电喷雾离子源正离子化后,通过三重四级杆串联质谱仪,采用选择反应监测(SRM)对齐拉西酮(m/z 413.2→194.1)和内标替米沙坦(m/z 515.3→276.2)进行测定,并用此法测定20例患者稳态血药浓度。结果齐拉西酮的高(250μg.L-1)、中(100μg.L-1)、低(10μg.L-1)3个质量浓度的平均回收率分别为100.33%,94.31%和104.70%,日内(n=5)、日间(n=3)RSD均小于15%;分析方法的最低定量限为5μg.L-1。线性范围为:5～500μg.L-1,回归方程为F=1.367 7ρ-0.024 5,r=0.999(n=7)。结论该方法灵敏、准确、简单、快速,可用于临床血浓监测和药动学研究。
Objective To establish a reversed-phase high performance liquid chromatography tandem mass spectrometry electrospray ionization (LC-ESI-MS / MS) method for the determination of ziprasidone in human plasma. Methods The mobile phase consisted of methanol-5 mmol.L-1 ammonium formate (90:10) at a flow rate of 1 mL on a C18 column (4.6 mm × 150 mm, 5 μm). min-1, column temperature: 25 ℃, with ethyl acetate - dichloromethane (4: 1) as extractant. The sample was electrospray ionized positive ionization, by triple quadrupole tandem mass spectrometer, selective reaction monitoring (SRM) on ziprasidone (m / z 413.2 → 194.1) and the internal standard telmisartan (m / z 515.3 → 276.2), and the steady-state plasma concentration of 20 patients was determined by this method. Results The average recoveries of ziprasidone at three concentrations of high (250μg.L-1), medium (100μg.L-1) and low (10μg.L-1) were 100.33%, 94.31% and 104.70% , Day (n = 5), daytime (n = 3) RSD less than 15%, and the lowest limit of quantitation of the assay was 5μg.L-1. The linear range was 5 ~ 500μg.L-1, the regression equation was F = 1.367 7ρ-0.024 5, r = 0.999 (n = 7). Conclusion The method is sensitive, accurate, simple and rapid and can be used in clinical blood concentration monitoring and pharmacokinetic studies.