高效液相色谱串联质谱法测定禽蛋中异丙嗪和氯丙嗪

Determination of Promethazine and Chlorpromazine in Poultry Eggs by High Performance Liquid Chromatography Tandem Mass Spectrometry

建立同时测定禽蛋中异丙嗪和氯丙嗪的高效液相色谱串联质谱(HPLC-MS/MS)法。样品以乙腈为提取剂,超声辅助提取,分散固相萃取进行净化,经ZORBAX Eclipse XDB-C18色谱柱(4.6 mm×50 mm,1.8μm)进行分离,在电喷雾电离(ESI)源正离子模式下,进行多反应监测(MRM),外标法定量。异丙嗪和氯丙嗪在0.5~100 ng/m L的浓度范围内线性关系良好,相关系数(r2)>0.999,检出限分别为0.05μg/kg和0.10μg/kg,定量限分别为0.17μg/kg和0.23μg/kg。在3个加标水平(10.0,20.0和100.0μg/kg)下,回收率为80.2%~102.0%,相对标准偏差(RSD)为2.5%~8.1%(n=7)。该方法简便、准确、灵敏,适用于禽蛋中异丙嗪和氯丙嗪的快速检测。

A method was developed for the simultaneous determination of promethazine and chlorpromazine in poultry eggs by high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS).The samples were ultrasonically extracted by acetonitrile,which was further purified by dispersive solid phase extraction,and the analytes were separated on a ZORBAX Eclipse XDB-C18 column(4.6 mm×50 mm,1.8μm),then detected by HPLC-MS/MS under multiple reaction monitoring(MRM)with positive ion mode of electrospray ionization(ESI),quantified by the external standard method.The calibration curves of promethazine and chlorpromazine were linear in the range of 0.5-100 ng/mL with good correlation coefficients(r2>0.999).For promethazine and chlorpromazine,the limits of detection were 0.05μg/kg and 0.10μg/kg,and the limits of quantification were 0.17μg/kg and 0.23μg/kg,respectively.The recoveries of promethazine and chlorpromazine at three spiked levels of 10.0,20.0 and 100.0μg/kg ranged from 80.2%to 102.0%with the relative standard deviations(RSD)of 2.5%-8.1%.The method was easy,accurate and sensitive,which could be applied in the rapid determination of promethazine and chlorpromazine in poultry eggs.