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目的建立测定人血浆中阿米舒必利浓度的高效液相色谱串联质谱电喷雾检测法(LC-MS/MS)。方法以WelchMaterials XB-C18(2.1mm×150mm,3μm)为色谱柱,流动相为甲醇-水(95∶5,含5mmol·L-1甲酸铵),流速为0.3mL·min-1,柱温:40℃,以乙酸乙酯-二氯甲烷(4∶1)为提取溶剂。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)对阿米舒必利(m/z370.3→242.1)和内标舒必利(m/z324.2→112.1)进行测定。结果阿米舒必利高(400μg·L-1)、中(250μg·L-1)、低(1.25μg·L-1)3个浓度的平均方法回收率分别为104.44%、104.74%和95.65%,日内(n=5)、日间(n=3)RSD均小于15%;分析方法的最低定量限为0.52μg·L-1。线性范围为:0.5～500μg·L-1。结论该方法灵敏、准确、简单、快速,可用于阿米舒必利临床血浓监测和药动学研究。
Objective To establish a liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for the determination of amisulpride in human plasma. Methods The column was WelchMaterials XB-C18 (2.1 mm × 150 mm, 3 μm). The mobile phase was methanol-water (95: 5, containing 5 mmol·L -1 ammonium formate) at a flow rate of 0.3 mL · min -1. : 40 ° C with ethyl acetate-dichloromethane (4: 1) as extraction solvent. Samples were electrospray ionized positive ionized by triple quadrupole tandem mass spectrometry, selective reaction monitoring (SRM) of amisulpride (m / z 370.3 -> 242.1) and the internal standard sulpiride (m / z 324.2 → 112.1). Results The average recoveries of the three concentrations of 400 mg · L-1, 250 μg · L-1 and 1.25 μg · L-1 were 104.44%, 104.74% and 95.65%, respectively. The RSDs were less than 15% during the day (n = 5) and day (n = 3). The lowest limit of quantification was 0.52 μg · L-1. The linear range is 0.5 ~ 500μg · L-1. Conclusion The method is sensitive, accurate, simple and rapid and can be used for clinical monitoring of blood concentration and pharmacokinetics of amisulpride.