色谱

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高效液相色谱-飞行时间质谱法筛查大豆中残留的多种除草剂和杀虫剂

储晓刚1,2,雍炜2,凌云2,姚惠源1,ZWEIGENBAUM Jerry3,方晏燕3

  

  1. 1.School of Food Science &Technology, Jiangnan University, Wuxi 214036, China;
    2.Institute of Food Safety, Chinese Academy of Inspection and Quarantine, Beijing 100025, China;
    3.Agilent Technologies Inc., Wilmington 19808-1610, USA
  • 收稿日期:2007-06-06 修回日期:2007-08-22 出版日期:2007-11-30 发布日期:1984-12-25
  • 通讯作者: 姚惠源

Screening Method for Multi Herbicide and Insecticide Residues in Soybeans Using High Performance Liquid Chromatography-Time-of-Flight Mass Spectrometry

CHU Xiaogang1,2, YONG Wei2, LING Yun2, YAO Huiyuan1, ZWEIGENBAUM Jerry3, FANG Yanyan3   

  1. 1.School of Food Science &Technology, Jiangnan University, Wuxi 214036, China;
    2.Institute of Food Safety, Chinese Academy of Inspection and Quarantine, Beijing 100025, China;
    3.Agilent Technologies Inc., Wilmington 19808-1610, USA
  • Received:2007-06-06 Revised:2007-08-22 Online:2007-11-30 Published:1984-12-25
  • Contact: YAO Huiyuan

摘要:

应用高效液相色谱-飞行时间质谱建立了筛查大豆中77种除草剂和杀虫剂残留的新方法。在不同添加浓度下获得了精确的分子离子质量,质量偏差的绝对值低于3×10-6。所有除草剂和杀虫剂在0.03~1.00 mg/kg范围内线性关系良好(r≥0.99)。除一些除草剂外,多数除草剂和杀虫剂的添加回收率为60%~120%,在大豆基质中的检测限为0.003~0.026 mg/kg。该方法适合于大豆中多种除草剂和杀虫剂残留的分析检测需要,方法简便、高效、准确。

关键词: 除草剂残留, 大豆 , 高效液相色谱-飞行时间质谱法, 杀虫剂残留, 筛查

Abstract:

A new multi-residue methodology using liquid chromatography-time-of-flight mass spectrometry (LC-TOF-MS) for the quantitative analysis of pesticides has been developed. The analytical performance of the method was evaluated by screening herbicide and insecticide residues in 10 kinds of imported soybeans. The accurate mass was obtained in different spiking levels (from 0.05 to 0.10 mg/kg) and the accuracy error was lower than 3×10-6, which is well within the accepted limits for target confirmation. The linearity of response ranged from 0.03 mg/kg to 1.0 mg/kg and the correlation coefficient was greater than 0.99. The average recoveries of herbicides and insecticides ranged from 60% to 120% of the fortified herbicides and insecticides in soybeans at 0.05-0.10 mg/kg levels for the majority of herbicides and insecticides, and the relative standard deviations (RSD) were between 2.17% and 13.54%. The limits of detection (LOD) were between 0.002 and 0.026 mg/kg. The results indicated that the method developed is easier, faster, and more sensitive. It also demonstrated that this method can meet the requirements for simultaneous determination of herbicides and insecticides in soybeans. This study provides valuable evidence for that LC-TOF-MS method has the potential in screening multi pesticide residues in soybeans.

Key words: insecticide residues, herbicide residues, screening, soybeans , high performance liquid chromatography-time-of-flight mass spectrometry (HPLC-TOF-MS)