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高效液相色谱-串联质谱快速测定饲料中硝基咪唑类药物及其代谢物残留

魏云计 丁涛 朱臻怡 冯民 何健 沈金荣 何正和 秦娴 张伶俐 钱怡平

分析测试学报2017,Vol.36Issue(3):377-381,5.
分析测试学报2017,Vol.36Issue(3):377-381,5.DOI:10.3969/j.issn.1004-4957.2017.03.014

高效液相色谱-串联质谱快速测定饲料中硝基咪唑类药物及其代谢物残留

Rapid Determination of Nitroimidazoles and Their Metabolites Residues in Feeds by High Performance Liquid Chromatography-Tandem Mass Spectrometry

魏云计 1丁涛 2朱臻怡 1冯民 1何健 1沈金荣 1何正和 1秦娴 1张伶俐 1钱怡平1

作者信息

  • 1. 淮安出入境检验检疫局国家饲料安全检测重点实验室(淮安),江苏淮安223001
  • 2. 江苏出入境检验检疫局动植物与食品检测中心,江苏南京210001
  • 折叠

摘要

Abstract

A high performance liquid chromatography-tandem mass spectrometric (HPLC-MS/MS) method was developed for the rapid determination of metronidazole (MNZ),metronidazole-OH (MNZOH),dimetridazole (DMZ),hydroxydimetridazole (HMMNI),ronidazole (RNZ),ipronidazole (IPZ),ipronidazole-OH(IPZOH) residues in feed.The samples were extracted with 0.1 mol/L pH 8.0 phosphate buffer and ethyl acetate-acetone (70 ∶ 30,by volume),then cleaned up with matrix solid-phase dispersant primary secondary amine (PSA).The extracts were defatted with hexane and cleaned up by liquid-liquid partition.The target compounds were detected by electrospray ionization (ESI) in positive mode using multiple reaction monitoring,and quantified by the isotope internal standard method.No solid-phase extract(SPE) procedure was adopted,which made sample preparation simple and efficient.The calibration curves for seven target compounds were linear in the range of 2.0-100.0 tμg/L with correlation coefficients more than 0.99.Average recoveries at spiked levels of 5.0-25.0 μ,g/kg were between 72.4% and 95.6%,with relative standard deviation less than 12.5%.The limits of detection(LOD) were 2.5 μg/kg,and the limits of quantitation(LOQ) were 5.0 μg/kg.

关键词

高效液相色谱-串联质谱/饲料/硝基咪唑类/代谢物

Key words

high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)/feed/nitroimidazoles/metabolites

分类

化学化工

引用本文复制引用

魏云计,丁涛,朱臻怡,冯民,何健,沈金荣,何正和,秦娴,张伶俐,钱怡平..高效液相色谱-串联质谱快速测定饲料中硝基咪唑类药物及其代谢物残留[J].分析测试学报,2017,36(3):377-381,5.

基金项目

质检总局科技计划项目(2015IK131) (2015IK131)

分析测试学报

OA北大核心CSCDCSTPCD

1004-4957

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