Determination of sedative drug residues in animal derived food by automatic SPE combined with ultra performance liquid chromatography-tandem mass spectrometry
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摘要: 建立全自动固相萃取-液质联用同位素内标法测定动物源性食品中13种镇静剂的方法。样品中添加同位素内标地西泮-d5和氯丙嗪-d6,经乙腈提取,全自动固相萃取仪净化,Waters ACQUITY UPLCTMBEH C18（2.1 mm×100 mm,1.7μm）不锈钢色谱柱分离,三重四级杆质谱多反应监测方式检测,同位素内标法定量。13种镇静剂在线性范围内具有良好的线性关系,相关系数r≥0.999,检出限在0.0300.113μg/kg之间,加标回收率在88.5%115.0%之间,相对标准偏差在2.45%7.92%之间。该方法样品前处理简单,净化过程实现了自动化操作,大大提高了工作效率;该方法灵敏度高、回收率好,适用于动物源性食品中多种镇静剂的同时检测。Abstract: A new approach for determination of 13 kinds of sedatives in animal derived food by automatic solid phase extration combined with ultra performance liquid chromatography- tandemmass spectrometry using isotope internal standard was described.The homogenized sample was spiked with diazepam- d5 and chlorpromazine- d6,and extracted with acetonitrile,then purified by automatic solid phase extration. After the analytes were separated by Waters ACQUITY UPLCTMBEH C18( 2.1 mm × 100 mm,1.7 μm) column.All sedatives were detected by MS/MS system with eletrospray ion ization( ESI+) under multiple reaction monitoring( MRM) mode and quantified by the isotope internal standard technique.The result indicated that the LOD of 13 kinds of sedatives ranged from 0.030μg / kg to 0.113 μg / kg.Meanwhile,the high correlation coefficents( r≥0.999) of 13 kinds of sedatives were obtained within their respective linear ranges. The average recoveries at low,intermediate and high spiked levels ranged from 88.5% to 115.0% with relative standard deviations( RSD) of 2.45% ~ 7.92%. The method with simple sample preparation achieved the automated purification process which then improved considerably the work efficiency.This method was suitable for simultaneous determination of multiple sedatives in animal derived food with simple pretreatment,high sensitivity,good recovery.
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Keywords:
- automatic solid phase extration /
- LC-MS / MS /
- animal derived food /
- sedatives
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