色谱

色谱 ›› 2019, Vol. 37 ›› Issue (10): 1042-1047.DOI: 10.3724/SP.J.1123.2019.04014

• 特别策划：固相萃取和QuEChERS应用专栏 • 上一篇    下一篇

QuEChERS-气相色谱-串联质谱法测定枸杞中农药残留

王芳焕, 任翠娟, 马辉, 李萍, 郝俊虎, 陈林, 孙敏   

  1. 银川海关技术中心, 宁夏 银川 750002
  • 收稿日期:2019-04-07 出版日期:2019-10-08 发布日期:2020-12-11
  • 通讯作者: 李萍,Tel:(0951)5661017,E-mail:55426066@qq.com.
  • 基金资助:
    宁夏回族自治区重点研发计划（2016KJHM131）.

Determination of pesticide residues in wolfberry using QuEChERS-gas chromatography-tandem mass spectrometry

WANG Fanghuan, REN Cuijuan, MA Hui, LI Ping, HAO Junhu, CHEN Lin, SUN Min   

  1. Yinchuan Customs Integrated Technology Center, Yinchuan 750002, China
  • Received:2019-04-07 Online:2019-10-08 Published:2020-12-11
  • Supported by:
    Ningxia Hui Autonomous Region Key Research and Development Project (No. 2016KJHM131).

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摘要： 建立了QuEChERS-气相色谱-串联质谱法测定枸杞中农药残留的分析方法。样品经乙腈提取，采用乙二胺-N-丙基硅烷（PSA）、C18和石墨化炭黑（GCB）3种吸附剂净化，在多反应监测模式（MRM）下进行检测，基质外标法定量。结果显示，检测项目在5~500 μg/L范围内呈良好线性（R2>0.99），在3个添加水平下测得回收率为71.5%~109.7%，相对标准偏差（RSD）为1.94%~9.87%（n=6）。该方法灵敏度高、净化效果好，可同时快速检测有机磷类、有机氯类农药。

关键词: QuEChERS, 气相色谱-串联质谱, 农药残留, 枸杞

Abstract: A method based on QuEChERS-gas chromatography-tandem mass spectrometry (GC-MS/MS) was established for the determination of 20 pesticide residues in wolfberry. The samples were extracted with acetonitrile. The extract was purified with PSA (primary secondary amine), GCB (graphite carbon black) and C18 to suppress the matrix in wolfberry. The analytical results showed that the calibration curves for the 20 pesticides obtained by GC-MS/MS were linear in the range of 5-500 μg/L, with the correlation coefficients higher than 0.99. The recoveries ranged from 70.02% to 110.78% with relative standard deviations (RSDs) ranging from 2.05% to 9.53%. This method has the advantages of being time-saving, convenient and sensitive. The proposed method can simultaneously detect organic phosphorus and organic chlorine pesticides residues with a good performance in terms of qualitative and quantitative detection.

Key words: QuEChERS, gas-chromatography-tandem mass spectrometry (GC-MS/MS), pesticide residues, wolfberry

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