UPLC-MS/MS检测生鲜牛奶中72种抗生素残留  

Determination of 72 antibiotics residues in raw milk by ultra-performance liquid chromatography-tandem mass spectrometry

作　　者：王承平[1,2] 秦宇 侯蓓蓓[1,2] 雷涛 虞成华 葛宇[1,2] WANG Cheng-ping;QIN Yu;HOU Bei-bei;LEI Tao;YU Cheng-hua;GE Yu(Shanghai Institute of Quality Inspection and Technical Research,Shanghai 200233,China;National Quality Supervision and Inspection Center for Food Products,Shanghai 200233,China)

机构地区：[1]上海市质量监督检验技术研究院,上海200233 [2]国家食品质量监督检验中心,上海200233

出　　处：《食品与机械》2019年第9期74-76,83,共4页Food and Machinery

基　　金：上海市科学技术委员会科研计划项目（编号：16391903800）

摘　　要：建立并优化了生鲜牛奶中抗生素残留的预处理方法,进行有效提取和净化,并使用超高效液相色谱-串联质谱仪对其进行分析。考察了不同提取溶剂和净化方式对5类72种化合物回收率的影响并优化了条件。结果表明,72种抗生素在1.0~100.0μg/L时线性关系良好;5种化合物LOD为10.0μg/kg,15种化合物LOD为5.0μg/kg,其余52种化合物LOD≤2.5μg/kg。72种抗生素加标回收率在低、中、高3个水平下分别为74.0%~118.8%,63.8%~122.6%,43.9%~139.7%,相对标准偏差分别为1.37%~29.61%,1.79%~30.27%,6.03%~39.70%。该方法灵敏度高,保留时间稳定,检测时间短,操作简便。The pretreatment method of antibiotic residues in fresh milk was established and optimized.At the same time,72 kinds of compounds were effectively extracted and purified,and analyzed by ultra performance liquid chromatography-tandem mass spectrometry.In this paper,the effects of different extraction solvents and purification methods on the recovery rate of the target were investigated and the conditions were optimized.72 antibiotics were linearly good in the range 1.0~100.0μg/L.The LOD of the five compounds was 10.0μg/kg,the LOD of the 15 compounds was 5.0μg/kg,and the LOD of the remaining 52 compounds was no more than 2.5μg/kg.The recoveries of 72 kinds of antibiotics were 74%~118.8%,63.8%~122.6%and 43.9%~139.7%,respectively,at low,medium and high levels,and the relative standard deviations were 1.37%~29.61%,1.79%~30.27%and 6.03%~39.70%.The method has good reproducibility,short detection time and simple operation,and provides a new rapid detection method for detecting antibiotic residues in fresh milk.

关 键 词：超高效液相色谱-串联质谱法 抗生素残留 生鲜牛奶 

分 类 号：R28[医药卫生—中药学]