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目的建立LC-MS/MS法测定药物左舒必利及起始原料中硫酸二甲酯的残留量。方法色谱柱采用Venusil XBP Phenyl column(100 mm×2.1 mm,5μm),流动相为100%甲醇,流速0.25 m L·min~(-1)。通过电喷雾离子化四级杆串联质谱,以多反应监测方式进行检测。结果硫酸二甲酯在质量浓度2.52~100.60μg·L~(-1)内线性关系良好,r2=0.997 5;在低、中、高浓度下的加样回收率分别为101.3%、103.9%及100.9%;方法精密度良好(RSD均<5%)。结论该方法快速、准确,适用于药物中微量硫酸二甲酯残留量的测定。
OBJECTIVE To establish a LC-MS / MS method for the determination of the drug residues in Zu-sulpiride and the residues of dimethyl sulfate in the starting materials. Methods The column was Venusil XBP Phenyl column (100 mm × 2.1 mm, 5 μm). The mobile phase consisted of 100% methanol and the flow rate was 0.25 m L · min -1. Electrospray ionization quadrupole mass tandem mass spectrometry, multi-reaction monitoring method for testing. Results The dimethyl sulfate showed good linearity (r2 = 0.997 5) in the range of 2.52 ~ 100.60 μg · L ~ (-1), and the recoveries were 101.3% and 103.9% at low, medium and high concentrations, respectively 100.9%. The method has good precision (RSD <5%). Conclusion The method is rapid and accurate and is suitable for the determination of traces of dimethyl sulfate in pharmaceuticals.