色谱

色谱 ›› 2019, Vol. 37 ›› Issue (1): 27-31.DOI: 10.3724/SP.J.1123.2018.10009

• 特别策划：南京海关动植物与食品检测中心专栏 • 上一篇    下一篇

气相色谱-负化学电离质谱法测定食用植物油中5种酰基吡唑类农药残留

沈伟健, 吴斌, 王红, 王晓研, 余可垚, 陆慧媛, 胡国绅, 李静静   

  1. 南京海关动植物与食品检测中心, 江苏 南京 210019
  • 收稿日期:2018-10-18 出版日期:2019-01-08 发布日期:2014-11-29
  • 通讯作者: 沈伟健E-mail:45467447@qq.com.
  • 基金资助:

    南京海关科研计划项目（2017KJ05，2018KJ38）.

Determination of five acylpyrazole pesticide residues in edible vegetable oils using gas chromatography-negative chemical ionization-mass spectrometry

SHEN Weijian, WU Bin, WANG Hong, WANG Xiaoyan, YU Keyao, LU Huiyuan, HU Guoshen, LI Jingjing   

  1. Animal, Plant and Food Inspection Center, Nanjing Customs, Nanjing 210019, China
  • Received:2018-10-18 Online:2019-01-08 Published:2014-11-29
  • Supported by:

    Nanjing Customs Research Project (Nos. 2017KJ05, 2018KJ38).

PDF

100

摘要：

建立了气相色谱-负化学电离质谱联用技术测定食用植物油中5种酰基吡唑类农药（呋吡菌胺、吡噻菌胺、氟唑菌苯胺、吡唑特、苄草唑）残留量的检测方法。样品经乙腈冷冻提取，分散固相萃取技术（QuEChERS）净化，采用基质校正曲线外标法定量。在20~1000 μg/L范围内，所有目标物的峰面积与其质量浓度均呈现良好的线性关系，定量限均低于2 μg/kg，能满足国内外的限量要求。在0.01、0.02、0.05 mg/kg 3个添加水平下，所有农药的平均回收率均处于82.7%~112.4%之间，相对标准偏差≤ 12.3%。该法准确度较高，精密度较好，灵敏度高，可用于食用植物油中酰基吡唑类农药残留量的测定。

关键词: 负化学电离, 气相色谱-质谱, 食用植物油, 酰基吡唑类农药

Abstract:

A method was established for the determination of five acylpyrazole pesticide residues in edible vegetable oils using gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS). The pesticides were extracted from a sample with acetonitrile under freezing conditions. A simple cleanup step known as QuEChERS was then conducted. After being identified by GC-NCI-MS, the extracts were quantified using an external standard method that employs a matrix correction standard curve. The linearity of the method was good between 20 and 1000 μg/L, and all limits of quantification were less than 2 μg/kg. Recoveries of all pesticides were in the range of 82.7%-112.4% at the three spiked levels of 0.01, 0.02, and 0.05 mg/kg, and all relative standard deviations were not more than 12.3%. Therefore, this method can be used to determine the residues of acylpyrazole pesticides in edible vegetable oils.

Key words: acylpyrazole pesticides, edible vegetable oils, gas chromatography-mass spectrometry (GC-MS), negative chemical ionization (NCI)

中图分类号: