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高效液相色谱-串联质谱法测定牛羊组织中苯酚类和水杨酸苯胺类抗蠕虫药多残留

李帅鹏 黄显会 王伟 严常燕 孔祥凯

分析化学2014,Vol.42Issue(3):423-428,6.
分析化学2014,Vol.42Issue(3):423-428,6.

高效液相色谱-串联质谱法测定牛羊组织中苯酚类和水杨酸苯胺类抗蠕虫药多残留

Simultaneous Determination of Phenolic and Salicylanilide Anthelmintics Multi-residues in Cattle and Ovine Tissues by HPLC-MS/MS

李帅鹏 1黄显会 1王伟 1严常燕 1孔祥凯1

作者信息

  • 1. 华南农业大学国家兽药残留基准实验室,广州510642
  • 折叠

摘要

Abstract

A high performance liquid chromatography-tandem mass spectrometric( HPLC-MS/MS) method was developed for the simultaneous determination of four phenolic and salicylanilide anthelmintics including nitroxinil, oxyclozanide, closantel and rafoxanide in cattle and ovine tissues. Muscle, liverand kidney were extracted with acetonitrile-acetone(60:40, V/V)and fat with 1% triethylamine in acetonitrile, then the extract was purified with MAX solid-phase extraction column. Qualitative and quantitative analysiswas achieved by HPLC-MS/MS undernegative multiple reaction monitoring ( MRM) mode. Good correlation coefficients were obtained (R>0. 99) in the concentration range of 1-100 μg/L. The limits of detection (LOD) and limits of qualification (LOQ) for the four compounds were 1 and 2. 5 μg/kg, respectively. The mean recoveries at the four levels of LOQ, 0. 5 maximum residue limit (MRL), MRL, 2MRL were between 71% and 112%,with the intra-day relative standard deviation(RSD)in the range of 1. 1%-14. 0%and inter-day RSD in the range of 6. 4%-14. 7%. Forty samples from the market were analyzed with the method, only two samples were found to show phenolic and salicylanilide anthelmintics residues.

关键词

苯酚类和水杨酸苯胺类抗蠕虫药/牛羊组织/多残留/高效液相色谱-串联质谱

Key words

Phenolic and salicylanilide anthelmintics/Cattle and ovine tissues/Multi-residues/High performance liquid chromatography-tandem mass spectrometry

引用本文复制引用

李帅鹏,黄显会,王伟,严常燕,孔祥凯..高效液相色谱-串联质谱法测定牛羊组织中苯酚类和水杨酸苯胺类抗蠕虫药多残留[J].分析化学,2014,42(3):423-428,6.

基金项目

本文系2012年农业行业标准制修订项目(No.201214148)资助 (No.201214148)

分析化学

OA北大核心CSCDCSTPCDSCI

0253-3820

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