毛细管柱气相色谱法测定中草药中8种有机氯农药残留

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。

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

Objective To establish the detective method of horganochlorine residues in herbs. Methods Organochlorine 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' - DDD and 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 5/μg/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%. Condnsion This method is simple, low cost and sensitive. The levels of 666 and DDT residues in four herbs are within permissible limits for herbs.