LC-MS/MS法测定人血浆中多潘立酮的浓度

Determination of Domperidone in Human Plasma by LC-MS-MS

目的:建立测定人血浆中多潘立酮浓度的高效液相-质谱联用色谱法。方法:以普萘洛尔为内标,血浆样本经0.1mol·L^(-1)氢氧化钠溶液处理后用乙醚萃取。采用XTerra MS C_(18)柱(150 mm×2.1 mm,3.5μm)为色谱柱,以乙腈-水-甲酸(80:20,含.3%的甲酸)为流动相,流速为0.2 ml·min^(-1)。质谱条件为电喷雾离子源(ESI),正离子方式多反应(MRM)扫描,离子选择通道分别为m/z 426.3→m/z 175.1(多潘立酮)和m/z 260.3→m/z 183.1(普萘洛尔)。结果:多潘立酮测定方法的线性范围为0.5～100μg·L^(-1),日内和日间精密度(RSD)均小于10%。结论:本方法特异性强,灵敏度高,适用于临床试验中血浆样本的高通量分析。

ABSTRACT Objective： To establish a liquid chromatography-tandem mass spectrometry （LC-MS-MS）method for the determination of domperidone in human plasma. Method： Propranolol was used as the internal standard. After alka/ified by 0. 1 mol· L ^- 1 NaOH, plasma was extracted by diethyl ether. Chromatography was performed on a XTerra MS C18 column with a mobile phase consisting of aeetonitrile-water-formie acid（ 80： 20：0.03 ）at a flow rate of 0.2 ml · min^-1. A triple quadrupole tandem mass spectrometer equipped with Turbo Ionspray Source was used as the detector and operated in the positive ion mode. Multiple reactions monitoring using the pre- cursor to produce ion combinations of m/z 426.3→m/z 175.1 and m/z 260.3→rm/z 183.1 was performed to quantify domperidone and the internal standard ambroxol, respectively. Result： The calibration curve of domperidone was linear within the range of 0.5-100μg ·L^-1. The intra- and inter-day RSDs were below 10%. Conclusion： LC-MS/MS method established in this study is simple and sensitive with promising accuracy, which is suitable to determine domperidone in plasma.