Wang Dong, Hou Chuanjin, Zhao Ercheng, Jia Chunhong
Se Pu. 2015 Jan;33(1):40-5. doi: 10.3724/sp.j.1123.2014.09022.
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 microg/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 microg/kg were 61.0%-100.1%, while the RSDs were 2.2%-19.5%. The limits of quantification for the eight pesticides were 20 microg/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.
建立了一种气相色谱 - 质谱联用（GC - MS）法测定蜂蜜中六氯环己烷（BHC）和滴滴涕（DDT）残留量，采用分散液液微萃取（DLLME）作为样品制备方法。样品用氯仿萃取，经涡旋和离心浓缩至氯仿中。通过GC - MS分析分析物。研究了影响萃取效率的因素，如萃取剂和分散剂的类型与体积、萃取时间等。同时评估了基质效应和方法性能。结果表明，由于基质效应，所有8种BHC和DDT农药均显示出信号增强。8种BHC和DDT农药的校准曲线在2 - 500μg/L范围内呈线性，相关系数为0.991 - 0.998。8种农药的富集因子（EF）为74 - 96。8种BHC和DDT农药在20、50和100μg/kg三个加标水平下的回收率为61.0% - 100.1%，相对标准偏差（RSD）为2.2% - 19.5%。8种农药的定量限为20μg/kg，检测限为1.0 ng。所建立的方法简便、快速且性能良好。适用于蜂蜜中BHC和DDT残留量的测定。
