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.
作者
陈楠楠
陈秀明
詹清
揭小玲
周阿容
方东升
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)
出处
《福建农业科技》
CAS
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)。
