色谱

色谱 ›› 2015, Vol. 33 ›› Issue (1): 40-45.DOI: 10.3724/SP.J.1123.2014.09022

• 研究论文 • 上一篇    下一篇

分散液液微萃取/气相色谱-质谱法测定蜂蜜中六六六和滴滴涕类农药残留

王东1,2, 侯传金1, 赵尔成2, 贾春虹2   

  1. 1. 大连工业大学轻工与化学工程学院, 辽宁 大连 116034;
    2. 北京市农林科学院植物保护环境保护研究所, 北京 100097
  • 收稿日期:2014-09-15 修回日期:2014-11-03 出版日期:2015-01-08 发布日期:2014-12-26
  • 通讯作者: 侯传金
  • 基金资助:

    国家自然科学基金资助项目(31301694);北京市农林科学院青年基金项目(QNJJ201310).

Determination of hexachlorocyclohexane and dichlorodi- phenyltrichloroethane residues in honey by gas chromatography-mass spectrometry combined with dispersive liquid-liquid microextraction

WANG Dong1,2, HOU Chuanjin1, ZHAO Ercheng2, JIA Chunhong2   

  1. 1. School of Light Industry and Chemical Engineering, Dalian Polytechnic University, Dalian 116034, China;
    2. Institute of Plant Protection and Environment Protection, Beijing Academy of Agriculture and Forestry Science, Beijing 100097, China
  • Received:2014-09-15 Revised:2014-11-03 Online:2015-01-08 Published:2014-12-26

PDF

214

被引次数

19

摘要：

建立了分散液液微萃取(DLLME)与气相色谱-质谱法(GC-MS)联用快速检测蜂蜜中六六六(BHC)和滴滴涕(DDT)类农药残留的分析方法.使用三氯甲烷为萃取剂,通过涡旋、离心使分析物富集到微量三氯甲烷中,采用气相色谱-质谱进行分析.实验对影响DLLME萃取效率的因素,如萃取剂种类和体积、分散剂种类和体积、萃取时间等进行了考察,同时对方法的基质效应和性能进行了评估.结果显示:由于基质效应,8种六六六和滴滴涕类农药都出现信号增强现象.8种六六六和滴滴涕类农药在2~500 μg/L范围内线性关系良好,相关系数(r2)为0.991~0.998,方法富集倍数为74~96;当试样的加标水平为20、50和100 μg/kg时,8种六六六和滴滴涕类农药的回收率为61.0%~100.1%,相对标准偏差(RSD, n=5)为2.2%~19.5%.8种六六六和滴滴涕类农药的最低检测浓度均为20 μg/kg,最小检出量皆为1.0 ng.该方法简单、快速、高效,适用于蜂蜜中六六六和滴滴涕类农药的残留检测.

关键词: 滴滴涕, 分散液液微萃取, 蜂蜜, 六六六, 气相色谱-质谱

Abstract:

A gas chromatography-mass spectrometry (GC-MS) method for the determination of hexachlorocyclohexane (BHC) and dichlorodiphenyltrichloroethane (DDT) residues in honey was developed using dispersive liquid-liquid microextraction (DLLME) as sample preparation method. The samples were extracted with chloroform, and concentrated into chloroform by vortex and centrifuging. The analytes were analyzed by GC-MS. The factors affecting the extraction efficiency were investigated, such as the type and volume of extraction and dispersive solvent, extraction time, etc. The matrix effects and method performance were evaluated at the same time. The results indicated that all the eight BHC and DDT pesticides displayed the enhancement of signals due to the matrix effects. The calibration curves were linear in the range of 2-500 μg/L and the correlation coefficients were 0.991-0.998 for the eight BHC and DDT pesticides. The enrichment factors (EF) were 74-96 for the eight pesticides. The recoveries of the eight BHC and DDT pesticides at three spiked levels of 20, 50 and 100 μg/kg were 61.0%-100.1%, while the RSDs were 2.2%-19.5%. The limits of quantification for the eight pesticides were 20 μg/kg, and the limits of detection were 1.0 ng. The developed method is easy, quick and with high performance. It is applicable for the determination of BHC and DDT residues in honey.

Key words: dichlorodiphenyltrichloroethane (DDT), dispersive liquid-liquid microextraction (DLLME), gas chromatography-mass spectrometry (GC-MS), hexachlorocyclohexane (BHC), honey

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