同位素内标-液质联用法检测猪肉中的苯二氮卓类药物残留  

Benzodiazepine drug residues detection in pork by ultra performance liquid chromatography-tandem mass spectrometry using isotope internal standard

作　　者：朱群英[1] 朱玉玲[1] 黄伟华[1] 索莉莉[1] 李良[1] 

机构地区：[1]南昌市疾病预防控制中心,江西南昌330038

出　　处：《现代预防医学》2017年第3期511-514,541,共5页Modern Preventive Medicine

基　　金：南昌市科技局(项目编号:洪科发计字【2013】210号第61项)

摘　　要：目的建立液质联用同位素内标法同时测定猪肉中硝西泮、氯硝西泮、氟硝西泮、奥沙西泮、劳拉西泮、阿普唑仑、替马西泮、地西泮的方法。方法在均质的猪肉样品中添加同位素内标地西泮-d5,经乙腈提取后用全自动固相萃取仪净化,液相色谱质谱联用仪检测,内标法定量。结果苯二氮卓类镇静剂药物在线性范围内具有良好的线性关系,线性相关性r≥0.999,检出限在0.030μg/kg^0.096μg/kg之间,加标回收率在89.8%-114.6%之间,相对标准偏差在2.45%~7.92%之间。结论该方法灵敏度高、回收率好,适用于猪肉中多种苯二氮卓类镇静剂药物残留的同时检测。Objective To establish a method for determination of nitrazepam, clonazepan,flunitrazepam, oxazepam, lorazepam, alprazolam, temazepam, diazepam in pork by ultra performance liquid chromatography - tandem mass spectrometry using isotope internal standard. Methods The homogenized pork sample was spiked with diazepam - d5 and extracted with acetonitrile,then purifying it by using automatic solid phase extraction apparatus. All benzodiazepine compounds were detected by LC - MS/MS system and quantified by the internal standard calibration curve of isotope dilution technique. Results The LODs of 8 benzodiazepine compounds ranged from 0. 030μg/kg to 0. 096μg/kg with the correlation coefficients greater than 0. 999. The average recoveries at low intermediate and high spiked levels ranged from 89.8 % to 114.6% with relative standard deviations （RSDs） of 2.45% - 7.92%. Conclusion The method is suitable for simultaneous determination of benzodiazepine drug residues in pork with simple pretreatment,high sensitivity,good recovery.

关 键 词：同位素内标 液质联用 猪肉 苯二氮卓类药物残留 

分 类 号：R115[医药卫生—公共卫生与预防医学]