色谱

色谱 ›› 2010, Vol. 28 ›› Issue (09): 840-848.DOI: 10.3724/SP.J.1123.2010.00840

• 研究论文 • 上一篇    下一篇

在线凝胶渗透色谱-气相色谱/质谱法检测茶叶中的153种农药残留

李军明*, 钟读波, 王亚琴, 冯雷, 祝红昆   

  1. 云南省产品质量监督检验研究院, 云南 昆明 650223
  • 收稿日期:2010-06-01 修回日期:2010-07-22 出版日期:2010-09-28 发布日期:2010-09-28
  • 通讯作者: 李军明,高级工程师.
  • 基金资助:

    国家质量监督检验检疫总局质检公益性行业科研专项课题(No. 200810498).

Determination of 153 pesticide residues in tea using on-line gel permeation chromatography-gas chromatography/mass spectrometry

LI  Junming*, ZHONG  Dubo, WANG  Yaqin, FENG  Lei, ZHU  Hongkun   

  1. Yunnan Product Quality Supervision and Testing Academy, Kunming 650223, China
  • Received:2010-06-01 Revised:2010-07-22 Online:2010-09-28 Published:2010-09-28

PDF

773

被引次数

73

摘要： 建立了在线凝胶渗透色谱-气相色谱/质谱(GPC-GC/MS)分析茶叶中153种农药残留的方法。样品用乙腈超声提取,提取液经石墨化炭黑固相萃取柱净化后,经GPC-GC/MS在线净化、分离和检测。方法的加标回收率为73.32%～117.05%,相对标准偏差为0.76%～13.18%。方法的检出限和定量限范围分别为0.0003～0.006 mg/kg和0.001～0.02 mg/kg。该方法样品前处理简单、分析时间短,灵敏度和精密度均符合农药多残留检测技术的要求,适用于茶叶中多种农药残留的检测。

关键词: 茶叶, 多农药残留, 气相色谱-质谱, 在线凝胶渗透色谱

Abstract: A method was developed for the determination of 153 pesticide residues in tea using on-line gel permeation chromatography-gas chromatography/mass spectrometry (GPC-GC/MS). The pesticide residues were extracted with acetonitrile under ultrasonic operation, and the extract was first cleaned up with an ENVI-carb solid phase extraction column and then separated and detected with the on-line GPC-GC/MS system. The recoveries of the method ranged from 73.32% to 117.05% with the relative standard deviations (RSDs) from 0.76% to 13.18%. The limits of detection and the limits of quantification were 0.0003~0.006 mg/kg and 0.001~0.02 mg/kg, respectively. This method is simple, rapid and characterized with acceptable sensitivity and accuracy to meet the requirements for the analysis of multiple pesticide residues in tea.

Key words: gas chromatography/mass spectrometry （GC/MS）, multiple pesticide residues, tea, on-line gel permeation chromatography (GPC)