色谱

色谱 ›› 2013, Vol. 31 ›› Issue (3): 218-222.DOI: 10.3724/SP.J.1123.2012.10003

• 研究论文 • 上一篇    下一篇

加速溶剂萃取-气相色谱-串联质谱法测定茶叶中10种吡唑和吡咯类农药的残留量

徐敦明1, 卢声宇2, 陈达捷1, 蓝锦昌2, 张志刚1, 杨方2, 周昱1*   

  1. 1. 厦门出入境检验检疫局, 福建 厦门 361026; 2. 福建出入境检验检疫局, 福建 福州 350001
  • 收稿日期:2012-10-10 修回日期:2013-01-22 出版日期:2013-03-28 发布日期:2013-03-22
  • 通讯作者: 杨方
  • 基金资助:

    厦门市科技计划项目(3502Z20092009,3502Z20102013);国家质检总局科技计划项目(2010IK192).

Determination of ten pesticides of pyrazoles and pyrroles in tea by accelerated solvent extraction coupled with gas chromatography-tandem mass spectrometry

XU Dunming1, LU Shengyu2, CHEN Dajie1, LAN Jinchang2, ZHANG Zhigang1, YANG Fang2, ZHOU Yu1*   

  1. 1. Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361026, China; 2. Fujian Entry-Exit Inspection and Quarantine Bureau, Fuzhou 350001, China
  • Received:2012-10-10 Revised:2013-01-22 Online:2013-03-28 Published:2013-03-22
  • Contact: YANG Fang

PDF

548

被引次数

70

摘要： 建立了加速溶剂萃取(ASE)-气相色谱-串联质谱(GC-MS/MS)法用于测定茶叶中10种吡唑和吡咯类农药残留。ASE萃取压力为1.03×107 Pa,萃取温度为100 ℃,萃取时间为5 min,萃取溶剂为乙酸乙酯-正己烷(1:1, v/v)。萃取循环1次,萃取液浓缩后用Envi-Carb/PSA固相萃取小柱净化,乙酸乙酯-正己烷(1:1, v/v)洗脱。洗脱液浓缩后,用正己烷定容,供GC-MS/MS测定,外标法定量。方法的准确度和精密度均符合残留分析要求。方法的定量限(LOQ)分别为唑螨酯0.003 mg/kg、氟虫腈硫化物0.001 mg/kg、氟虫腈0.002 mg/kg、氟虫腈砜化物0.005 mg/kg、溴虫腈0.002 mg/kg、氟硅唑0.006 mg/kg、野燕枯0.001 mg/kg、吡草醚0.001 mg/kg、吡螨胺0.0003 mg/kg、唑虫酰胺0.005 mg/kg。方法的灵敏度能满足各国有关农药的残留限量要求。

关键词: 吡咯, 吡唑, 残留分析, 加速溶剂萃取, 农药, 气相色谱-串联质谱

Abstract: An effective method was developed and applied to determine the residues of ten pesticides of pyrazoles and pyrroles in tea by accelerated solvent extraction coupled with gas chromatography-tandem mass spectrometry (ASE-GC-MS/MS). The samples were extracted with ethyl acetate-hexane(1:1, v/v) for 5 min at 1.03×107 Pa and 100 ℃ for one cycle. Then, they were purified by Envi-Carb/PSA column, and eluted by ethyl acetate-hexane (1:1, v/v). The analytes were determined by GC-MS/MS and quantified by external standard method. The limits of quantification were 0.003 mg/kg for fenpyroximate, 0.001 mg/kg for fipronil-sulfide, 0.002 mg/kg for fipronil, 0.005 mg/kg for fipronil-sulfone, 0.002 mg/kg for chlorfenapyr, 0.006 mg/kg for flusilazole, 0.001 mg/kg for difenzoquat, 0.001 mg/kg for pyraflufen-ethyl, 0.0003 mg/kg for tebufenpyrad and 0.005 mg/kg for tolfenpyrad. The results show that the proposed method is sensitive and accurate for the determination of the ten pesticide residues.

Key words: gas chromatography-tandem mass spectrometry (GC-MS/MS), pesticide, pyrazole, pyrrole, residue analysis, accelerated solvent extraction (ASE)