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

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.