超滤型高脂基质净化柱结合超高效液相色谱-三重四极杆液质联用法测定鱼肉中七种镇静剂  

Determination of seven kinds of sedative drugs in fish by MPFC-QuEChERS combined with UPLC-MS/MS

作　　者：王小乔 李坚 许晓辉 石晓峰 吴福祥[1] 张生萍 邵长春 张虹艳 潘秀丽 李赟 WANG Xiaoqiao;LI Jian;XU Xiaohui;SHI Xiaofeng;WU Fuxiang;ZHANG Shengping;SHAO Changchun;ZHANG Hongyan;PAN Xiuli;LI Yun(Lanzhou Institute for Food and Drug Control/Key Laboratory of Pesticides and Veterinary Drugs Monitoring for State Market Regulation,Lanzhou 730050,China;Gansu Provincial Academic Institute for Medical Research,Lanzhou 730050,China;College of Pharmacy,Gansu University of Chinese Medicine,Lanzhou 730000,China)

机构地区：[1]兰州市食品药品检验检测研究院/国家市场监管重点实验室(食品中农药兽药残留监控),甘肃兰州730050 [2]甘肃省医学科学研究院,甘肃兰州730050 [3]甘肃中医药大学药学院,甘肃兰州730000

出　　处：《食品与发酵工业》2023年第24期267-274,共8页Food and Fermentation Industries

基　　金：甘肃省市场监督管理局科技计划资助(SSCJG-SP-A202204);甘肃省市场监督管理局科技计划资助(SSCJG-SP-202104)。

摘　　要：该研究旨在建立同时测定鱼肉中7种苯二氮卓类镇静催眠药(咪达唑仑、艾司唑仑、硝西泮、阿普唑仑、氯硝西泮、三唑仑、地西泮)的分析方法。样品经乙腈提取和兽药残留专用萃取盐包(内含1 g氯化钠和4 g硫酸钠)萃取,提取液通过超滤型高脂基质净化柱(multiplug filtration clean-up-QuEChERS,MPFC-QuEChERS)净化;采用超高效液相色谱-三重四极杆液质联用法(ultra-performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)外标法定量测定供试品中7种苯二氮卓类镇静催眠药。结果显示,7种镇静催眠药在0~20 ng/mL内线性良好,相关系数大于0.99,检出限(S/N=3)和定量限(S/N=10)分别为0.25~2.0μg/kg和1.0~4.0μg/kg,加标回收率和相对标准偏差分别为83.8%~114.2%和1.1%~8.7%。表明该方法操作简单,准确可靠,适用于同时测定鱼肉中7种苯二氮卓类镇静催眠药。The analytical method of simultaneous determination of seven kinds of sedative drugs in fish was established,seven kinds of sedative drugs included midazolam,eszolam,nitrazepam,alprazolam,clonazepam,triazolam,and diazepam.The samples were extracted by acetonitrile and a special extraction salt pack of Agilent Bond Elut QuEChERS,and the extraction solution was purified by a purification column of MPFC-QuEChERS.Seven kinds of benzodiazepine sedative and hypnotic drugs were determined by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS),and quantified by external standard method.Results showed that the calibration curves of seven kinds of sedative drugs showed good linearity in the concentration range of 0-20 ng/mL with correlation coefficients not less than 0.99.The limits of detection(S/N=3)and limits of quantitation(S/N=10)were 0.25-2.0μg/kg and 1.0-4.0μg/kg,respectively.The recoveries for seven kinds of sedative drugs at three spiked levels ranged from 83.8%to 114.2%with relative standard deviations of 1.1%-8.7%.The method is simple,accurate and reliable,and is suitable for simultaneous quantitative determination of seven kinds of benzodiazepine sedative and hypnotic drugs in fish.

关 键 词：鱼肉 镇静催眠药 提取净化 测定 MPFC-QuEChERS UPLC-MS/MS 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]