色谱

色谱 ›› 0, Vol. ›› Issue (): 0-0.DOI: 10.3724/SP.J.1123.2013.01034

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LC-Q-TOF/MS快速筛查与确证苹果、西红柿和卷心菜中281种农药残留

赵志远1,2,范春林2   

  1. 1. 河北大学
    2. 中国检验检疫科学研究院
  • 收稿日期:2013-01-17 修回日期:2013-01-26 出版日期:2013-02-04 发布日期:2013-02-04
  • 通讯作者: 范春林

Rapid screening and confirmation of 281 pesticides residue in Apple, Tomato and Cabbage by LC-Q-TOF/MS

Zhi-Yuan ZHAO,   

  • Received:2013-01-17 Revised:2013-01-26 Online:2013-02-04 Published:2013-02-04

摘要： 摘要：建立了苹果、西红柿和卷心菜中281种农药残留QuEChERS结合LC-Q-TOF/MS快速筛查方法。方法采用20 mL 1%醋酸乙腈振荡提取，醋酸钠与无水硫酸镁盐析后，经丙基乙二胺（PSA）吸附剂净化， LC-Q-TOF/MS测定。281种农药在苹果、西红柿和卷心菜3个添加水平下，回收率在70%~120%范围的比例分别为98.6%、99.3%和98.2%；相对标准偏差（RSD）均≤20%（n=5）；在0.25~10MRL范围内，281种农药线性相关系数r2≥0.99的农药比例分别为95.7%、96.1%和98.2%；检出限分别为0.03~4.47 μg/kg，0.01~4.49 μg/kg和0.02~3.61 μg/kg。方法能够满足各国农药残留限量的要求。本方法采用LC-TOF数据库和LC-Q-TOF数据库检索的方式，实现了不用农药标准品对照，完成对果蔬中多类农药残留的快速筛查，不仅提高了方法定性鉴别的准确性，而且节省了购买标准品的成本。应用本方法对30个市售果蔬样品进行筛查，共检出13种农药残留，其中包括杀菌剂、杀螨剂及杀虫剂。采用基质匹配外标校准曲线进行定量，卷心菜中甲胺磷的浓度超过了《GB 2763-2012食品安全国家标准 食品中农药最大残留限量》欧盟最大残留限量(MRLs)，西红柿中鱼藤酮含量超出了MRLs.

Abstract: Abstract: The application of QuEChERS coupled to LC-Q-TOF/MS for screening 281 pesticides in apple, tomato and cabbage has been investigated. The established method includes extraction by 20 mL of acetonitrile/acetic acid (99+1, v/v), salting out by adding sodium acetate and magnesium sulfate, cleanup by PSA sorbent. The residue is detected by LC-Q-TOF/MS. For apple, tomato and cabbage, the percentages of compounds with the average recoveries (n=5) in the range of 70%~120% are 98.6%, 99.3% and 98.2%, respectively; and the relative standard deviations (RSDs) are lower than 20%; in the level of 0.25~10 MRL, the percentages of compounds with the correlation coefficients (r2)≥0.99 are 95.7%, 96.1% and 98.2%, respectively; LOD are 0.03~4.47 μg/kg, 0.01~4.49 μg/kg and 0.02~3.61 μg/kg, respectively. The method adopt of TOF and Q-TOF database search to achieve the purpose of rapid screening and confirmation. The method has been applied to 30 fruit and vegetable samples purchased from market, and the results show that 17 pesticides are detected. These pesticides belong to antiseptic, acaricide and insecticide. The matrix-matched external calibration has been used for quantification. The methamidophos in a cabbage exceed the 《GB 2763-2012 National food safety standard Maximum residue limits for pesticides in food》and the maximum residue limits (MRLs) from European Union (EU). The concentration of rotenone in a tomato sample exceed MRLs from European Union (EU).

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