色谱 ›› 2018, Vol. 36 ›› Issue (12): 1211-1222.DOI: 10.3724/SP.J.1123.2018.09012

• 研究论文 • 上一篇    下一篇

QuEChERS-液相色谱-串联质谱法测定蔬菜中105种农药残留

邓慧芬, 张建莹, 黄科, 钟恬恬, 林丽敏   

  1. 深圳海关食品检验检疫技术中心, 广东 深圳 518045
  • 收稿日期:2018-09-06 出版日期:2018-12-08 发布日期:2014-11-06
  • 通讯作者: 张建莹,Tel:(0755)26680670,E-mail:zhangjianying1001@163.com
  • 基金资助:

    原国家质检总局项目(2017IK271,2017IK262).

Determination of 105 pesticide residues in vegetables by QuEChERS-liquid chromatography-tandem mass spectrometry

DENG Huifen, ZHANG Jianying, HUANG Ke, ZHONG Tiantian, LIN Limin   

  1. Food Inspection & Quarantine Center, Shenzhen Customs, Shenzhen 518045, China
  • Received:2018-09-06 Online:2018-12-08 Published:2014-11-06
  • Supported by:

    Former General Administration of Quality Supervision, Inspection and Quarantine Project (Nos. 2017IK271, 2017IK262).

摘要:

通过优化QuEChERS前处理方法并结合液相色谱-串联质谱(LC-MS/MS)技术建立了蔬菜中105种典型杀虫剂、杀菌剂、除草剂、植物生长调节剂的多残留测定方法。目标化合物使用乙腈提取,以150 mg乙二胺-N-丙基硅烷(PSA)、150 mg封端十八烷基键合硅胶吸附剂(EC-C18)、30 mg石墨化炭黑(GCB)作为基质提取液净化剂。实验结果表明,在0.010~0.200 mg/L范围内,105种目标化合物的线性相关系数(r)>0.99,方法定量限为0.010 mg/kg;3个添加水平的回收率范围为68.2%~108%,相对标准偏差(RSD)为1.02%~11.8%。该方法快速简便,净化效果好,可用于蔬菜中日常农药残留的测定。

关键词: QuEChERS, 农药残留, 蔬菜, 液相色谱-串联质谱

Abstract:

After optimization of the QuEChERS pretreatment method, combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS) technology, a multi-residue determination method was established for 105 typical insecticides, bactericides, herbicides, and plant growth regulators in vegetables. The target compounds were extracted by acetonitrile, purified with 150 mg primary secondary amine (PSA), 150 mg EC-C18, and 30 mg graphitized carbon black (GCB) adsorbents. The standard curves of 105 target compounds were linear in the concentration range of 0.010-0.200 mg/L, with correlation coefficients (r)>0.99. The limit of quantification was 0.010 mg/kg, the recoveries were between 68.2% and 108% at three spiked levels, and the RSDs of the method were between 1.02% and 11.8%. The method is suitable for the rapid determination of the common pesticides in vegetables owing to its advantages of rapidity, simplicity, and better purification.

Key words: liquid chromatography-tandem mass spectrometry (LC-MS/MS), pesticide residues, QuEChERS, vegetables

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