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中国农学通报

中国农学通报 ›› 2017, Vol. 33 ›› Issue (26): 128-135.doi: 10.11924/j.issn.1000-6850.casb16080104

所属专题： 水产渔业

• 水产 渔业 • 上一篇    下一篇

分散固相萃取-超高液相色谱/质谱测定水产品中磺胺类抗生素的残留量

余丽梅   

  1. 中国水产科学研究院淡水渔业研究中心
  • 收稿日期:2016-08-23 修回日期:2017-09-05 接受日期:2016-12-21 出版日期:2017-09-19 发布日期:2017-09-19
  • 通讯作者: 余丽梅
  • 基金资助:
    2016 年度国家水产品质量安全风险评估项目“国家水产品质量安全风险评估”(GJFP2016)。

Dispersive Solid-phase Extraction-Ultra Performance Liquid Chromatography Tandem Mass Spectrometry Detecting Sulfonamides Residues in Aquatic Products

  • Received:2016-08-23 Revised:2017-09-05 Accepted:2016-12-21 Online:2017-09-19 Published:2017-09-19

摘要： 为了更快、更准、更简易地测定水产品中磺胺类抗生素的残留量，建立了分散固相萃取(dSPE)-超高液相色谱/质谱(UPLC-MS/MS)测定水产品中磺胺类抗生素残留量的方法。实验主要比较了3种样品净化方法：分散固相萃取(dSPE)法、旋转蒸发浓缩法、国家标准净化方法。处理的水产样品，稀释后经UPLC-MS/MS进行检测分析。结果表明，分散固相萃取(dSPE)法对样品前处理比其他2种方法快速，精确，简易。经分散固相萃取(dSPE)法净化后的磺胺类药物在0.5~50 μg/L浓度范围内线性关系良好，相关系数均大于0.9；仪器检出限为0.0007~0.002 μg/L，方法的检出限为0.007~0.02 μg/kg，定量限为0.02~0.08 μg/kg。在水产品中的加标回收率为67.0%~173.5%，RSD为2%~24.5%。该方法实现了快速、简单、准确地测定水产品中磺胺类抗生素残留分析，为研究水产品中磺胺类抗生素残留快速准确检测的方法提供参考。

关键词: 遥感, 遥感, 参数反演, 地表温度, MERSI, MODIS, RSD

Abstract: In order to more fast, easily and precisely detecting sulfonamides residues in aquatic products, dispersive solid phase extraction (dSPE)-ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was established. Three methods of purification, including dSPE, rotary evaporation condensation and the national standard purified method, were compared in this study. Aquatic samples were detected by UPLC-MS/MS after dilution. The results showed that dSPE was more fast, accurate and simple in dealing with aquatic samples than the other two methods. The calibration curves for selected sulfonamides (concentration range of 0.5~50 μg/L) were linear with correlation coefficients more than 0.9. Detection limits of instrument and method were 0.0007~0.002 μg/L and 0.007~0.02 μg/kg respectively. And limits of quantitation ranged from 0.02 μg/kg to 0.08 μg/kg. The recovery and RSD were 67.0%~173.5% and 2%~24.5% respectively. In a word, this method is fast, simple and accurate, can be developed for detecting and analyzing sulfonamides residues, and also provides a reference for research of fast and accurately detecting sulfonamides residues.