Florisil固相萃取-气相色谱法测定蜂蜜中的六六六、滴滴涕残留量

Determination of hexachlorocyclohexane and dichlorodiphenyl trichloroethane in honey by florisil solid phase extraction-gas chromatography

中文关键词:  气相色谱法  蜂蜜  六六六  滴滴涕  Florisil固相萃取

英文关键词:gas chromatography  honey  hexachlorocyclohexane  dichlorodiphenyl trichloroethane  florisil solid phase extraction

中文摘要:

      目的 建立Florisil固相萃取-气相色谱法测定蜂蜜中六六六(hexachlorocyclohexane, HCH)、滴滴涕(dichlorodiphenyl trichloroethane, DDT)残留量的分析方法。方法 样品加水后利用乙腈提取残留农药, 选用Florisil柱中加入乙二胺-Ｎ-丙基硅烷(primary secondary amine, PSA)为净化材料, 以固相萃取方法净化样品, 以DB-17石英毛细管色谱柱分离, 采用气相色谱-电子捕获检测器测定, 以峰面积外标法定量。结果 8种农药在3个添加水平下的平均回收率在70.2%~97.4%之间, 相对标准偏差为1.2%~9.6%, 方法检出限为0.00006~0.0004 mg/kg, 均能达到农残分析的要求。结论 该方法具有操作简便、快速、准确的特点, 适用于蜂蜜中六六六、滴滴涕残留的分析。

英文摘要:

      Objective To establish a method for determination of hexachlorocyclohexane (HCH) and dichlorodiphenyl trichloroethane (DDT) in honey by florisil solid phase extraction-gas chromatography. Methods The pesticides were extracted by acetonitrile after adding water, cleaned-up by solid phase extraction with florisil column added primary secondary amine (PSA), separated by the capillary columns of DB-17, detected by gas chromatography with electron capture detector(GC-ECD), and quantified by the external standard method. Results At different spiked levels, the average recoveries of 8 kinds of pesticides were in the range of 70.2%~97.4% with the relative standard deviations of 1.2%~9.6%, the limits of detection of the method were 0.00006~0.0004 mg/kg, which could meet the requirements for the analysis of pesticide residues. Conclusions This method is simple, rapid and accurate, and can be used for the analysis of HCH and DDT in honey.