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)

作　　者：马宁 李洪波 张振宇 黄志伟 赵盼盼 MA Ning;LI Hong-bo;ZHANG Zhen-yu;HUANG Zhi-wei;ZHAO Pan-pan(Zhumadian Product Quality Inspection and Testing Center,Zhumadian 463000,China;Product Quality Inspection and Testing Center of Jiyuan Production City Integration Demonstration Zone,Jiyuan 459000,China)

机构地区：[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

出　　处：《粮食与饲料工业》2024年第6期66-71,共6页Cereal & Feed Industry

基　　金：河南省济源市科技攻关项目(23021004)。

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0.5~10.0μg/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0.1μg/kg,定量限为0.5μg/kg。在1.0、2.5、5.0μg/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。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 spectrometry(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 pretreatment conditions and GC/MS(gas chromatography-mass spectrometry)conditions,chloramphenicol drugs presented good linearity(r>0.9990)within the mass concentration of 0.5-10.0μg/L.The detection limit was 0.1μg/kg,while the quantification limit was 0.5μg/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 1.0μg/kg,2.5μg/kg,and 5.0μg/kg.The method features simple pretreatment procedures,fast analysis,and high precision,which proves its applicability to screening and quantitative analysis of chloramphenicol drugs in feeds.

关 键 词：Prime HLB UPLC-MS/MS 氯霉素类 饲料检测 

分 类 号：S816.17[农业科学—饲料科学]