高等学校化学学报

高等学校化学学报 ›› 2006, Vol. 27 ›› Issue (2): 227.

• 研究论文 • 上一篇    下一篇


气质联机分析蔬菜中农药多残留及基质效应的补偿

黄宝勇1,2, 潘灿平1, 王一茹3, 曹喆3, 张微1, 李文明1, 江树人1   

  1. 1. 中国农业大学理学院应用化学系, 北京 100094;  2. 北京市农业环境监测站, 北京 100026;
    3. 安捷伦公司亚太区北京环境分析实验室, 北京 100083
  • 收稿日期:2005-04-08 出版日期:2006-02-10 发布日期:2006-02-10
  • 通讯作者: 潘灿平(1970年出生), 男, 博士, 副教授, 博士生导师, 主要从事农药残留与环境毒理方面的研究. E-mail:canpingp@cau.edu.cn
  • 基金资助:

    国家重点基础研究发展规划(批准号: 2002CB410805)资助.

Rapid Determination of Pesticide Multiresidues in Vegetable by Gas Chromatography\|mass  Spectrometry and Compensation for Matrix Effect with Protectants

HUANG Bao-Yong 1,2, PAN Can-Ping1, WANG Yi-Ru3, CAO Zhe3,
ZHANG Wei1, LI Wen-Ming1, JIANG Shu-Ren1   

  1. 1. Department of Applied Chemistry , College of Science, China Agricultural University, Beijing 100094, China;
    2. Beijing Station of Agro\|Environmental Monitoring, Beijing 100029, China;
    3. Beijing Environmental Analysis Lab, Asia\|Pacific Region, Agilent Technologies, Beijing 100083, China
  • Received:2005-04-08 Online:2006-02-10 Published:2006-02-10
  • Contact: PAN Can-Bing,E-mail:canpingp@cau.edu.cn

PDF (PC)

摘要：

摘要建立了蔬菜中52种农药化合物的气相色谱\|质谱检测方法, 考察了基质效应和分析保护剂在方法中的应用, 评价了3种分析保护剂组合的加入对补偿基质效应的影响, 确定了最佳配比. 样品前处理采用乙腈提取, 用PSA(Primary-secondary amine)固相材料分散净化技术, 用气质联机在选择离子监测模式下分析检测. 该方法在0.01～1.00 mg/L范围内线性关系良好, 相关系数大于0.98, 最低检测浓度除溴氰菊酯和异菌脲外均在0.2～9.4 mg/kg之间, 各化合物添加回收率为81.8%～119.5%, 相对标准偏差为0.8%～17.6%.

关键词: 关键词基质效应; 农药多残留; 气相色谱-质谱法; 分析保护剂

Abstract:

Abstract A multi-residue method is described for rapid determination of 52 multi-class pesticides, including  their isomers, in vegetables by gas chromatography-mass spectrometry(GC-MS) with the aid of analyte protectants. Addition of different  combinations of  protectants before injection for compensation of matrix effect was demonstrated. Pesticides were extracted from samples with acetonitrile and the extract was cleaned up by using dispersive method by primary-secondary amine sorbent. Pesticides was injected into GC with the aid of analyte protectants [3-ethoxy-1,2-propanediol(20 mg/mL)and D-sorbitol(1 mg/mL)] , followed by MS detection under EI ionization and selective ion monitoring mode. Good linear and lower limits of detection were obtained, the linear range are between 0.01 and 1.00 mg/L, correlation coefficients are better than 0.98, and the detection limits are mainly between 0.2 and 9.4 μg/kg. All compounds have mean recoveries of 81.8%-119.5% and the relative standard deviation is between 0.8% and 17.6%.

Key words: KeywordsMatrix effect; Multi\, residue of pesticide; Gas chromatography-mass spectrometry(GC-MS); Analyte protectants

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