超高效液相色谱-质谱对动物源食品中氯丙嗪、异丙嗪及其代谢物的测定  

Determination of Chlorpromazine and Promethazine and Their Metabolites in Animal Food Using Ultra Performance Liquid Chromatography with Tandem Mass Spectrometry

作　　者：齐士林[1] 吴敏[2] 严丽娟[2] 吴抒怀[2] 邹伟[2] 林立毅[2] 周昱[2] 

机构地区：[1]厦门大学化学系,福建厦门361002 [2]厦门出入境检验检疫局,福建厦门361026

出　　处：《分析测试学报》2009年第6期677-681,共5页Journal of Instrumental Analysis

基　　金：国家质量监督检验检疫总局科研计划资助项目(2007IK137)

摘　　要：建立了动物源食品中吩噻嗪类药物氯丙嗪、异丙嗪及其代谢物氯丙嗪亚砜和异丙嗪亚砜同时测定的固相萃取超高效液相色谱-电喷雾电离串联四极杆质潜（UPLC—ESI MS／MS）方法样品用乙酸乙酯和氢氧化钠溶液提取，Oasis HLB柱富集净化，超高效液相色潜-电喷雾串联四极杆质谱仪检测，采用多反应监测正离子模式，可以一次性对动物源性食品中的吩噻嗪类药物氯丙嗪、异丙嗪及其代谢物氯丙嗪亚砜和异丙嗪亚砜进行定性和定量测定一方法在1～100μg／L范围具有良好的线性，回收率为76％～96％，定量下限（S／N〉10）为异丙嗪5μg/kg,氯丙嗪、氯丙嗪亚砜、异丙嗪亚砜1μg/kg。检出限（S／N=3）为异丙嗪1．5μg/kg，氯丙嗪、氯丙嗪亚砜、异丙嗪亚砜0．3μg／kg。A method for the simultaneous detection residues of chlorpromazine and promethazine and their metabolites chlorpromazine sulphoxide and promethazine sulphoxide in animal foods was developed by using solid phase extraction （SPE） combination with ultra performance liquid chromatography - electrospray ionization triple-quadruple tandem mass spectrometry.（ UPLC -ESI MS/MS）. The chlorpromazine and promethazine and their metabolites in the test sample was extracted with ethyl acetate and sodium hydroxide solution. The homogenate was centrifuged and the supernatant was collected. The extract was cleaned up and concentrated on an Oasis HLB cartridge, and then analyzed by UPLC - ESI MS/MS under the positive ion mode using multiple reaction monitoring（MRM） mode. Extraction and chromatographic conditions were optimized and the best separation was obtained. The cabalibration curves were linear in the range of 1 - 100 μg/L. The average recoveries were between 76% and 96% （n =6） in the spiked range of 5 - 100 μg/kg in pork, fish, dullfrog and milk. The limits of quantification（S/N 〉 10） were in the range of 1 -5 μg/kg and the limits of detection （S/N = 3 ） were 0. 3 - 1.5 μg/kg.

关 键 词：固相萃取 超高效液相色谱-电喷雾电离质谱 氯丙嗪 异丙嗪 氯丙嗪亚砜 异丙嗪亚砜 动物源性食品 

分 类 号：O657.63[理学—分析化学] S859.84[理学—化学]