食品与发酵工业 >

2023 , Vol. 49 >Issue 24: 267 - 274

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.036099

分析与检测

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

  • 王小乔 ,
  • 李坚 ,
  • 许晓辉 ,
  • 石晓峰 ,
  • 吴福祥 ,
  • 张生萍 ,
  • 邵长春 ,
  • 张虹艳 ,
  • 潘秀丽 ,
  • 李赟
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  • 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)
第一作者:学士,高级工程师(石晓峰主任药师和张生萍高级工程师为共同通信作者,E-mail:shixiaofeng2005@sina.com;1043577029@qq.com)

收稿日期: 2023-05-10

  修回日期: 2023-08-15

  网络出版日期: 2024-01-17

基金资助

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)

收起

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

  • WANG Xiaoqiao ,
  • LI Jian ,
  • XU Xiaohui ,
  • SHI Xiaofeng ,
  • WU Fuxiang ,
  • ZHANG Shengping ,
  • SHAO Changchun ,
  • ZHANG Hongyan ,
  • PAN Xiuli ,
  • LI Yun
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  • 1(Lanzhou Institute for Food and Drug Control/Key Laboratory of Pesticides and Veterinary Drugs Monitoring for State Market Regulation, Lanzhou 730050, China)
    2(Gansu Provincial Academic Institute for Medical Research, Lanzhou 730050, China)
    3(College of Pharmacy, Gansu University of Chinese Medicine, Lanzhou 730000, China)

Received date: 2023-05-10

  Revised date: 2023-08-15

  Online published: 2024-01-17

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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0.25～2.0 μg/kg和1.0～4.0 μg/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。

关键词： 鱼肉; 镇静催眠药; 提取净化; 测定; MPFC-QuEChERS; UPLC-MS/MS

本文引用格式

王小乔 , 李坚 , 许晓辉 , 石晓峰 , 吴福祥 , 张生萍 , 邵长春 , 张虹艳 , 潘秀丽 , 李赟 . 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[J]. 食品与发酵工业, 2023 , 49(24) : 267 -274 . DOI: 10.13995/j.cnki.11-1802/ts.036099

Abstract

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 0.25-2.0 μg/kg and 1.0-4.0 μg/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.

Key words： fish; sedative and hypnotic drugs; extraction and purification; determination; MPFC-QuEChERS; UPLC-MS/MS

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