QuEChERS结合高效液相色谱串联质谱法检测猪肉中16种兽药残留量  

Determination of 16 Kinds of Veterinary Drug Residues in Pork by QuEChERS Coupled with HPLC-MS/MS

作　　者：陈楠楠 陈秀明[1] 詹清 揭小玲 周阿容 方东升[1] CHEN Nan-nan;CHEN Xiu-ming;ZHAN Qing;JIE Xiao-ling;ZHOU A-rong;FANG Dong-sheng(Fujian Institute of Microbiology,Fuzhou,Fujian 350007,China)

机构地区：[1]福建省微生物研究所,福建福州350007

出　　处：《福建农业科技》2024年第9期51-58,共8页Fujian Agricultural Science and Technology

基　　金：福建省科技计划省属公益类项目(2020R1005008、2022R10050010)。

摘　　要：建立了一种QuEChERS前处理与高效液相色谱串联质谱法(HPLC-MS/MS)相结合同时检测猪肉中16种兽药残留的方法。样品采用水−0.1%甲酸乙腈经QuEChERS技术提取和净化后,在正离子多反应监测模式(multiple reaction monitoring,MRM)下进行分析测定。结果表明:16种兽药在2.0~100.0μg·kg^(−1)的范围内有良好的线性关系(相关系数r>0.9970);检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)的范围分别为0.01~0.25μg·kg^(−1)、0.03~0.82μg·kg^(−1);在猪肉样品中进行了2、4、20μg·kg^(−1)3个不同浓度水平的加标试验,相对标准偏差RSD为1.1%~9.0%,加标回收率在70.4%~118.1%。该方法的重复性和回收率满足试验要求,灵敏度高,适用于猪肉中多种类兽药残留的分析检测。A method for the simultaneous determination of 16 veterinary drug residues in pork by using QuEChERS pretreatment combined with high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)was established.The samples were extracted and purified by using the QuEChERS technology with water−0.1%formic acid acetonitrile,and then analyzed and determined in the positive ion multiple reaction monitoring(MRM)model.The results showed that:there was a good linear relationship among the 16 veterinary drugs in the range of 2.0−100.0μg·kg^(−1)(the correlation coefficient r>0.9970).The limits of determination(LOD,S/N=3)and limits of quantitation(LOQ,S/N=10)ranged from 0.01 to 0.25μg·kg^(−1)and from 0.03 to 0.82μg·kg^(−1),respectively.The spiked experiments at three different concentration levels of 2,4 and 20μg·kg^(−1)were carried out in the pork samples.The relative standard deviation(RSD)ranged from 1.1%to 9.0%,and the recovery rate ranged from 70.4%to 118.1%.The repeatability and recovery rate of the method met the test requirements,and the sensitivity was high,which was suitable for the analysis and detection of various veterinary drug residues in pork.

关 键 词：兽药残留 猪肉 高效液相色谱-串联质谱(HPLC-MS/MS) QUECHERS 

分 类 号：S859.84[农业科学—临床兽医学]