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中国精品科技期刊2020
谭高好,王承业,郑金明,等. UPLC-MS/MS法同时测定动物源性食品中37种兽药残留[J]. 食品工业科技,2021,42(17):225−234. doi: 10.13386/j.issn1002-0306.202009030.
引用本文: 谭高好,王承业,郑金明,等. UPLC-MS/MS法同时测定动物源性食品中37种兽药残留[J]. 食品工业科技,2021,42(17):225−234. doi: 10.13386/j.issn1002-0306.202009030.
TAN Gaohao, WANG Chengye, ZHENG Jinming, et al. Simultaneous Determination of 37 Veterinary Drugs in Animal-Derived Foods by Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry(UPLC-MS/MS)[J]. Science and Technology of Food Industry, 2021, 42(17): 225−234. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.202009030.
Citation: TAN Gaohao, WANG Chengye, ZHENG Jinming, et al. Simultaneous Determination of 37 Veterinary Drugs in Animal-Derived Foods by Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry(UPLC-MS/MS)[J]. Science and Technology of Food Industry, 2021, 42(17): 225−234. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.202009030.

UPLC-MS/MS法同时测定动物源性食品中37种兽药残留

Simultaneous Determination of 37 Veterinary Drugs in Animal-Derived Foods by Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry(UPLC-MS/MS)

  • 摘要: 建立了QuEChERS净化结合超高效液相色谱-串联质谱(UPLC-MS/MS)法同时测定动物源性食品中37种兽药残留量的分析方法。样品经1%甲酸/乙腈沉淀蛋白提取,N-丙基乙二胺(PSA)、C18吸附剂、NH2吸附剂净化后;然后,通过Waters ACQUITY UPLC BEH C18(1.7 μm,2.1 mm×100 mm)色谱柱分离,采用0.1%甲酸/水溶液-甲醇为流动相进行梯度洗脱;电喷雾正离子模式电离,采用多反应监测模式(MRM)检测,基质匹配标准曲线外标法定量。结果表明,37种目标物在1.0~200 μg/L范围内线性相关系数(r)均在0.9980以上。在3个不同浓度添加水平下,样品回收率在70.1%~97.7%之间,方法RSD为0.9%~5.6%,定量限(S/N≥10)为0.01~0.54 μg/kg。采用本方法对农贸市场购买的152批动物源性食品样品进行检测,3批罗非鱼均检出磺胺嘧啶和甲氧苄氨嘧啶,其余样品均未检出。该方法操作简便、快速,具有良好的精密度、准确度和定量限,适用于动物性食品中硝基咪唑类及其代谢物和磺胺类的快速检测。

     

    Abstract: A method for the determination of 37 veterinary drugs in animal-derived foods with QuEChERS by UPLC-MS /MS was established. The sample was extracted by 1% formic acid-acetonitrile precipitated protein, purified by PSA, C18, NH2 adsorbent. The separation was performed on Waters ACQUITY UPLC BEH C18 (1.7 μm, 2.1 mm×100 mm) column. The mobile phase performed on 0.1% formic acid aqueous solution-methanol by gradient elution, electrospray ionization source (ESI) was applied and operated in the positive mode. Multiple reaction monitoring (MRM) mode was used to monitor ions. Matrix matching standard curve quantification by external standard method. Results showed that, an excellent linear relationship in the range of 1.0~200 μg/L was observed for all the analytes with a correlation coefficient larger than 0.9980. The recoveries at three concentrations ranged from 70.1% to 97.7%, with the RSD from 0.9% to 5.6%. The limits of quantification of the method were 0.01~0.54 μg/kg. This method was used to detect 152 batches of animal-derived food samples which purchased at the farmer’s market. Sulfadiazine and trimethoprim were detected in 3 batches of Oreochromis mossambicus, the remaining samples were not detected. The method was simple, rapid and had good precision, accuracy and quantitative limit. It would be suitable for the rapid determination of nitroimidazoles and their metabolites, sulfonamides in animal-derived foods.

     

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