双水相-超高效液相色谱串联质谱法测定猪肉中17种抗生素  

Determination of 17 antibiotics in pork by aqueous two-phase extraction combined with ultra-high performance liquid chromatography-tandem mass spectrometry

作　　者：李雨薇 张洪昌 胡双庆 李贞金 沈根祥[1,2] 赵晓祥 LI Yuwei;ZHANG Hongchang;HU Shuangqing;LI Zhenjin;SHEN Genxiang;ZHAO Xiaoxiang(College of Environmental Science and Engineering,Donghua University,Shanghai 201620,China;State Environmental Protection Key Laboratory of Environmental Health Impact Assessment of Emerging Contaminants,Shanghai Academy of Environmental Sciences,Shanghai 200233,China)

机构地区：[1]东华大学环境科学与工程学院,上海201620 [2]上海市环境科学研究院国家环境保护新型污染物环境健康影响评价重点实验室,上海200233

出　　处：《东华大学学报（自然科学版）》2023年第2期159-166,共8页Journal of Donghua University(Natural Science)

基　　金：上海市科技兴农项目(沪农科推字(2020)第1-4号)。

摘　　要：为了解上海地区市售猪肉中抗生素残留水平,对猪肉中抗生素的分析方法进行了筛选与优化。选择双水相方法,对提取液和分相盐进行了筛选优化,建立了猪肉中5类17种典型抗生素的分析方法,并检测了上海地区市售猪肉中抗生素的残留水平。结果表明:采用双水相结合超高效液相色谱串联质谱法,选择质量分数为0.2%的甲酸-乙腈/乙二胺四乙酸二钠(Na_(2)-EDTA)作为提取溶剂,(NH_(4))_(2)SO_(4)作为分相盐时,17种目标抗生素的加标回收率最佳,回收率为65.3%~129.7%,相对标准偏差小于12.6%,检出限和定量限分别为0.04~5.51μg/L和0.14~18.35μg/L;上海地区市售猪肉样品均未检出17种抗生素。研究表明,该分析方法能满足猪肉样品中痕量抗生素的检测残留要求,且具有选择性好、灵敏度高的优点,适合猪肉中17种抗生素的残留检测。To understand the residual antibiotic levels in commercial pork in Shanghai,the analytical method of antibiotics in pork was screened and optimized.The aqueous two-phase extraction was selected,and the extraction solution and layered salt were screened and optimized to establish the analytical method for 5 categories of 17 typical antibiotics in pork,and the residue levels of antibiotics in commercial pork samples in Shanghai were detected.Results show that the recoveries of the 17 target antibiotics are 65.3%-129.7%with the relative standard deviations less than 12.6%,and the limits of detection and limits of quantification are 0.04-5.51μg/L and 0.14-18.35μg/L,respectively,when the method of aqueous two-phase extraction combined with ultra-high performance liquid chromatographytandem mass spectrometry selects 0.2%formic acid-acetonitrile/disodium ethylenediaminetetraacetic acid(Na_(2)-EDTA)as the extraction solvent and(NH_(4))_(2)SO_(4)as layered salt.Seventeen antibiotics are not detected in commercial pork in Shanghai.The study shows that this analytical method can meet the requirements of the trace antibiotics residue detection in pork samples,which is good selectivity,high sensitivity,and suitable for the detection of 17 antibiotic residues in pork.

关 键 词：猪肉 抗生素 超高效液相色谱串联质谱法 双水相 

分 类 号：X830.2[环境科学与工程—环境工程]