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中国精品科技期刊2020
吴彦蕾,苏敏,周纯洁,等. QuEChERS-超高效液相色谱-串联质谱法同时检测猪肉中76种兽药及其代谢物[J]. 食品工业科技,2023,44(20):311−321. doi: 10.13386/j.issn1002-0306.2022110330.
引用本文: 吴彦蕾,苏敏,周纯洁,等. QuEChERS-超高效液相色谱-串联质谱法同时检测猪肉中76种兽药及其代谢物[J]. 食品工业科技,2023,44(20):311−321. doi: 10.13386/j.issn1002-0306.2022110330.
WU Yanlei, SU Min, ZHOU Chunjie, et al. Simultaneous Determination of 76 Veterinary Drugs and Their Metabolites in Pork by QuEChERS-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2023, 44(20): 311−321. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2022110330.
Citation: WU Yanlei, SU Min, ZHOU Chunjie, et al. Simultaneous Determination of 76 Veterinary Drugs and Their Metabolites in Pork by QuEChERS-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2023, 44(20): 311−321. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2022110330.

QuEChERS-超高效液相色谱-串联质谱法同时检测猪肉中76种兽药及其代谢物

Simultaneous Determination of 76 Veterinary Drugs and Their Metabolites in Pork by QuEChERS-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

  • 摘要: 为提高猪肉中多兽药残留检测的效率,建立了QuEChERS结合超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定猪肉中5类76种兽药及其代谢物残留量的方法,包括喹诺酮类、磺胺类、硝基咪唑类、大环内酯类、苯并咪唑类。样品经酸化乙腈提取,无水硫酸钠盐析,提取液经C18和无水硫酸镁净化后分为两部分,一部分用于22种弱极性化合物的直接测定,另一部分氮吹浓缩后复溶,用于54种强极性化合物的测定。76种化合物均采用电喷雾电离正离子模式多反应监测(MRM),基质匹配外标法定量分析。结果表明,76种兽药及其代谢物线性关系良好,相关系数均大于0.995,方法定量限均低于10 μg/kg,加标回收率为61.3%~96.2%,相对标准偏差(RSD)为2.0%~14.6%。方法应用于170批市售猪肉,其中23批次样品检出2类5种兽药残留。该方法简便快速、准确可靠,适用于猪肉中多类兽药残留的快速筛查和精准检测。

     

    Abstract: In order to improve the efficiency of the detection of multiple veterinary drug residues in pork, a method for the simultaneous determination of 5 types of 76 veterinary drugs and their metabolites residues in pork, including quinolones, sulfonamides, nitroimidazoles, macrolides and benzimidazoles, was established by QuEChERS combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were extracted with acidified acetonitrile and salted out by anhydrous sodium sulfate. The extract was divided into two parts after purified by C18 and anhydrous magnesium sulfate. One part was used for direct determination of the 22 weakly polar compounds, and the other part was concentrated by nitrogen blowing for the determination of the 54 strongly polar compounds. The 76 compounds were analyzed in multiple reaction monitoring (MRM) mode via electrospray ionization, and quantified by matrix matching external standard method. The results showed that the correlation coefficients were greater than 0.995, and the limits of quantification (LOQs) were lower than 10 μg/kg. The recoveries ranged from 61.3% to 96.2%, with the relative standard deviation (RSD) between 2.0% and 14.6%. The method was applied to 170 pork samples sold in the market, 23 samples of which were detected with 2 types of 5 veterinary drugs residues. The method was simple, rapid, accurate, reliable, and suitable for rapid screening and accurate detection of multiple veterinary drug residues in pork.

     

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