色谱

色谱 ›› 2010, Vol. 28 ›› Issue (12): 1162-1167.DOI: 10.3724/SP.J.1123.2010.01162

• 研究论文 • 上一篇    下一篇

气相色谱法检测22种基质中的4种二硫代氨基甲酸盐类农药残留

秦曙1,2, 乔雄梧2*, 王霞2, 赵丽娟2   

  1. 1. 山西大学黄土高原研究所, 山西 太原 030006; 2. 山西省农业科学院山西省农药重点实验室, 山西 太原 030031
  • 收稿日期:2010-08-19 修回日期:2010-10-25 出版日期:2010-12-28 发布日期:2010-08-28
  • 通讯作者: 乔雄梧,博士,研究员,主要研究方向为农药环境毒理学. Tel: (0351)7581865, E-mail: qiaoxiongwu@126.com.
  • 基金资助:

    山西省重点实验室开放基金项目(Nos. 200503013, 200603014, 2009011059-6).

Determination of 4 dithiocarbamate residues in 22 matrices by gas chromatography

QIN Shu1,2, QIAO Xiongwu2*, WANG Xia2, ZHAO Lijuan2   

  1. 1. Institute of Loess Plateau, Shanxi university, Taiyuan 030006, China| 2. Shanxi Key Laboratory of Pesticide Science, Shanxi Academy of Agricultural Sciences, Taiyuan 030031, China
  • Received:2010-08-19 Revised:2010-10-25 Online:2010-12-28 Published:2010-08-28

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1011

被引次数

25

摘要： 在密闭加热的容器中用SnCl2-HCl溶液酸解二硫代氨基甲酸盐类（DTCs）农药,反应生成的二硫化碳气体被瓶中的正己烷吸收,形成二硫化碳的正己烷溶液;使用气相色谱-火焰光度检测器(硫滤光片)测定有机相中二硫化碳的含量,即得到DTC农药的残留量。采用该方法对苹果、葡萄等22种基质中残留的代森锰锌、代森联、丙森锌和福美双进行了方法确证: 添加水平为0.06～3.0 mg/kg时,平均回收率为72%～110%,相对标准偏差为0.8%～22.0%,采用外标法定量,方法的检出限范围为0.01～0.1 mg/kg(信噪比(S/N)为3),定量限范围为0.02～0.2 mg/kg(S/N=10)。该方法简单、快速、准确、重复性好,适用于不同基质中DTCs农药的残留检测。

关键词: 残留, 二硫代氨基甲酸盐农药, 气相色谱, 蔬菜；水果；植物；土壤

Abstract: A gas chromatographic method with flame photometric detection (FPD (sulfur filter)) for analyzing the residues of 4 dithiocarbamates in 22 matrices in a heated closed vial has been established. The dithiocarbamate residues were decomposed to carbon disulfide (CS2) by SnCl2-HCl solution. The liberated CS2 was absorbed by hexane in the vial, and then determined by gas chromatography with FPD (sulfur filter). The results were expressed as the residues of dithiocabamates. The residue analysis method was validated by mancozeb, metiram, propineb and thiram in 22 matrices (apple, grape, etc). The average recovery ranges were from 72% to 110% with the relative standard deviations (RSD) between 0.8% and 22.0% when the fortified concentrations were between 0.06 and 3.0 mg/kg, and the quantitative analysis was performed by using external standard method. The limits of detection were in the range of 0.01~0.1 mg/kg (S/N=3), and the limits of quantification were between 0.02 and 0.2 mg/kg (S/N=10) for the 4 dithiocarbamate residues in the 22 matrices. This method is simple, fast, accurate, reproducible, and suitable for the determination of the 4 dithiocarbamate residues in the matrices mentioned in this paper.

Key words: dithiocarbamate pesticides, fruit, plant, residues, soil, vegetable, gas chromatography (GC)