毛细管气相色谱测定中成药中20种有机氯农药的残留量

Determination of organochlorine pesticide residues in Chinese patent medicine by CGC

目的建立了7种中成药中20种有机氯农药残留[六六六(α-BHC,β-BHC,γ-BHC和δ-BHC 4种异构体),滴滴涕(pp'-DDE,pp'-DDD,pp'-DDT和op'-DDT 4种同系物),五氯硝基苯、艾试剂、七氯、环氧七氯、异狄氏剂、狄氏剂、六氯苯、五氯苯胺、五氯甲基苯硫醚、顺氯丹、反氯丹、氧氯丹]的GC-ECD测定方法。方法采用乙酸乙酯超声提取并经固相萃取柱及硫酸净化杂质,用DB-1701P弹性石英毛细管柱分离待测组分,ECD检测器进行检测。进样口温度260℃,检测器温度300℃,柱升温程序(初始温度130℃,3℃/min升至160℃,1℃/min升至170℃,保持18 min,再以6℃/min升至220℃,保持8 min),柱流量1.0 mL/min,不分流进样,进样量1μL。结果 20种有机氯农药线性回归方程的相关系数在0.997 9～0.999 9范围之内,线性关系良好,方法的平均回收率为78.4%～119.8%,RSD为1.3%～6.2%。结论本方法快速、简便、准确,适用于中成药中20种有机氯类农药多组分残留的检测。

AIM To develop a capillary gas chromatography to determine the residues of twenty organochlorine pesticides [benzene hexachloride（α-BHC,β-BHC,γ-BHC,δ-BHC）,DDT（pp′-DDE,pp′-DDD,pp′-DDT,op′-DDT）,PCNB,aldrin,heptachlor,heptachlor epoxide,endrin,dieldrin,hexachlorobenzene,pentachlorophenol aniline,methyl-pentachlorophenyl sulfide,cis-chlordane,trans-chlordane,oxy-chlordane] in seven kinds of traditional Chinese patent medicine.METHODS The samples were extracted with ethyl acetate by ultrasonic,then cleaned up by a column packed with florisil and then treated with sulfuric acid to remove the inpurites.The capillary column was DB-1701P（30 m×0.32 mm,0.25 μm） with electron capture detector.The injector temperature was 260 ℃ and the detector temperature was 300 ℃.The column temperature program was initial temperature 130 ℃,with the increase rate of 3 ℃ per min to 160 ℃,1 ℃ per min to 170 ℃（held 18 min）,6 ℃ per min to 220 ℃（held 8 min）.The pesticide residues were calculated by external standard method.RESULTS The related coefficients were from 0.997 9 to 0.999 9.The average recoveries and RSDs were in the ranges of 78.4%-119.8% and 1.3%-6.2%.CONCLUSION The method is rapid,simple and accurate.It can be used to determine organochlorine pesticide residues in traditional Chinese patent medicine.