食品科学 ›› 2011, Vol. 32 ›› Issue (8): 278-280.doi: 10.7506/spkx1002-6630-201108063

• 分析检测 • 上一篇    下一篇

超高效液相色谱质谱联用仪测定水产品中敌百虫的含量

查玉兵,杨春亮*,林 玲,李 涛,程盛华   

  1. 中国热带农业科学院农产品加工研究所
  • 出版日期:2011-04-25 发布日期:2011-04-12

Determination of Trichlorphon Residues in Aquatic Products Using UPLC-MS/MS

ZHA Yu-bing,YANG Chun-liang*,LIN Ling,LI Tao,CHENG Sheng-hua   

  1. 1. Agricultural Products Processing Research Institute, Chinese Academy of Tropical Agricultural Sciences, Zhanjiang 524001, China
  • Online:2011-04-25 Published:2011-04-12

摘要: 建立敌百虫在水产品中残留量的超高效液相色谱-电喷雾质谱(UPLC-MS/MS)测定方法。用乙酸乙酯提取样品中的敌百虫,提取液经酸性氧化铝柱净化,经超高效液相色谱分离,用串联质谱测定,正离子多反应监测(MRM)模式检测,外标法定量。在0.02~0.8ng/mL范围内,敌百虫标准工作溶液的色谱峰面积与质量浓度成良好的线性关系,相关系数r=0.9992;水产品中敌百虫的添加回收率在89.0%~93.8%,相对标准偏差为2.1%~5.4%,检出限为1.0μg/kg。方法简便、快速、准确,保留时间为1.5min。

关键词: 敌百虫, 残留, 液相色谱-质谱/质谱联用仪, 水产品

Abstract: A UPLC-MS/MS method was developed to determine trichlorphon residues in aquatic products. Trichlorphon residues in samples were extracted into ethyl acetate, defatted on an acidic alumina solid phase extraction column, separated by UPLC, measured by MS/MS in positive ion multiple reaction monitoring mode, and quantified by external standard method. Over the range of 0.02 to 0.8 ng/mL, an excellent linear relationship (r = 0.9992) between trichlorphon concentration and peak area was observed for the standard working solution of trichlorphon. The average spike recoveries for trichlorphon in blank samples ranged from 89.0 % to 93.8 %, with a RSD between 2.1% and 5.4%. The detection limit for trichlorphon was 1μg/kg. This method proved simple, rapid and accurate.

Key words: UPLC-MS/MS, trichlorfon, aquatic products, residues

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