毛细管柱气相色谱法测定中草药中8种有机氯农药残留

DETERMINATION OF HUMAN SERUM ORGANOCHLORINE RESIDUES BY GAS CHROMATOGRAPHY EQUIPPED WITH ELECTRON CAPTURE DETECTOR

目的建立中草药中8种有机氯农药残留的气相色谱分析方法,为中草药中有机氯残留检测提供有效的技术手段。方法样品采用正己烷:石油醚:丙酮(V:V:V,2:2:1)萃取4h,超声波震荡提取30min,过氟罗里硅土层析柱净化,80℃水浴蒸发近干,GC-ECD检测分析。结果对样品前处理条件进行优化,采用DB-5石英毛细管柱分离样品,GC-ECD测定8种有机氯残留,8种有机氯农药残留组分在25min内能够很好的分离,其质量浓度与色谱峰面积在0.01～5.00μg/ml的浓度范围内呈线性关系,检出限<0.02μg/ml。该方法二个水平的加标回收率是83.4%～115.6%,RSD是2.1%～7.3%。结论该方法简便成本低,准确度高,利用该方法检测的4种中草药样品中的六六六(HCH)和滴滴涕(DDT)残留均未超标。

Objective To establish the detective method of horganochlorine residues in herbs. Methods Organochlorine residues in herb were extracted ultrasonically with hexane., petroleum ether： acetone （V ： V ： V：2 ： 2 ： 1）, clean- up with Florisil chromatographic column, concentrated and determined by gas chromatography with electron capture detector （ECD）. Results α-HCH, β-HCH,γ-HCH,δ-HCH,P,P-DDE,O,P -DDT, P, P＇-DDDand P, P＇- DDT can be separated within 25 min under optimized condition. The linear range between peak area and concentration of organochlorine residues concentration was from 0.02μg/ml to 5μg/ml. The limit of detection was less than 0.02μg/ml （S/N = 3）. The recovery was from 81.5% to 117.6%. RSD was from 2. 1% to 7.3%. Conclusion This method is simple, low cost and sensitive. The levels of 666 and DDT residues in four herbs are within permissible limits for herbs.