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  

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

作　　者：王东[1,2] 侯传金[1] 赵尔成[2] 贾春虹[2] 

机构地区：[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

出　　处：《色谱》2015年第1期40-45,共6页Chinese Journal of Chromatography

基　　金：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)

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2-500μg／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100μg／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20μg／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。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 extrac-tion efficiency were investigated,such as the type and volume of extraction and dispersive sol-vent,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 recover-ies 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＆amp;nbsp;easy,quick and with high performance. It is applicable for the determination of BHC and DDT residues in honey.

关 键 词：分散液液微萃取 气相色谱-质谱 六六六 滴滴涕 蜂蜜 

分 类 号：O658[理学—分析化学]