粮食与饲料工业2024,Issue(6) :66-71.DOI:10.7633/j.issn.1003-6202.2024.06.016

基于通过式固相萃取柱-UPLC-MS/MS快速测定饲料中氯霉素类药物

Rapid determination of chloramphenicol drugs in feeds with pass-through solid phase extraction column and ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)

马宁 李洪波 张振宇 黄志伟 赵盼盼
粮食与饲料工业2024,Issue(6) :66-71.DOI:10.7633/j.issn.1003-6202.2024.06.016

基于通过式固相萃取柱-UPLC-MS/MS快速测定饲料中氯霉素类药物

Rapid determination of chloramphenicol drugs in feeds with pass-through solid phase extraction column and ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)

马宁 1李洪波 1张振宇 2黄志伟 1赵盼盼1
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作者信息

  • 1. 驻马店市产品质量检验检测中心,河南驻马店 463000
  • 2. 济源产城融合示范区检验检测中心,河南济源 459000
  • 折叠

摘要

研究旨在建立Prime HLB快速净化前处理技术结合UPLC-MS/MS测定饲料中氯霉素类药物的检测分析方法.饲料样品经乙腈提取,Prime HLB固相萃取柱一步式净化,UPLC-MS/MS MRM监测模式,采用乙腈-水系统作为流动相梯度洗脱,ESI-模式下进行检测分析,基质内标法定量.在充分优化前处理条件和色谱质谱条件下,氯霉素类药物在质量浓度为0.5~10.0 μg/L的线性范围内,呈现良好的线性关系(r>0.999 0),方法检出限为0.1 µg/kg,定量限为0.5 μg/kg.在1.0、2.5、5.0 µg/kg样品加标水平下的平均回收率在93.1%~103.2%,相对标准偏差(n=5)不大于3.1%.该方法前处理步骤简单,分析速度快,准确度高,可用于饲料中氯霉素类药物的筛查和定量分析.

Abstract

This study aimed to establish an approach for rapidly detecting and analyzing chloramphenicol drugs in feeds by combing Prime HLB fast-purifying pretreatment technology with ultra performance liquid chromatography tandem mass spec-trometry(UPLC-MS/MS).Extracted with acetonitrile,feed samples went through further purification in Prime HLB solid-phase extraction column,gradient elution with acetonitrile-water as mobile phase in the monitoring mode of UPLC-MS/MS MRM and analytical test in ESI mode.The substrate was quantified using internal standard method.Under fully optimized pre-treatment conditions and GC/MS(gas chromatography-mass spectrometry)conditions,chloramphenicol drugs presented good linearity(r>0.999 0)within the mass concentration of 0.5-10.0 μg/L.The detection limit was 0.1 μg/kg,while the quanti-fication limit was 0.5 μg/kg.The average recovery rate ranged from 93.1%to 103.2%,and the relative standard deviation(n=5)was no higher than 3.1%when samples were added at 1.0 μg/kg,2.5 μg/kg,and 5.0 μg/kg.The method features simple pretreatment procedures,fast analysis,and high precision,which proves its applicability to screening and quantitative a-nalysis of chloramphenicol drugs in feeds.

关键词

Prime/HLB/UPLC-MS/MS/氯霉素类/饲料检测

Key words

Prime HLB/UPLC-MS/MS/chloramphenicol drugs/feeds detection

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出版年

2024
粮食与饲料工业
国家粮食储备局 武汉科学研究设计院

粮食与饲料工业

CSTPCD
影响因子:0.513
ISSN:1003-6202
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