黔产5种中药材有机氯农药残留安全限量研究

Safety limits of organochlorine pesticide residues in five kinds of Chinese herbal medicines from Guizhou

目的:对5种黔产中药材中总六六六(α-BHC、β-BHC、γ-BHC、δ-BHC)、总滴滴涕(p,p′-DDE、p,p′-DDD、o,p′-DDT、p,p′-DDT)和五氯硝基苯(PCNB)的9种有机氯农药残留量进行测定,为控制中药材安全限量提供实验数据,为开发利用药材资源提供安全性保障。方法:样品经丙酮,二氯甲烷与石油醚混合有机溶剂超声提取,选用气相色谱-电子捕获检测(GC-ECD)Rtx-1701弹性石英毛细管柱(0.25 mm×30 mm×0.25μm),以不分流方式进样,进样口温度230℃,检测器温度300℃;程序升温,初始温度100℃,先以10℃/min升至220℃,再以8℃/min升至250℃保持10 min,外标法计算含量,应用SPSS 22.0软件对数据结果进行统计学分析。结果:9种有机氯的线性关系良好,相关系数均大于0.995;最低检出限为0.00012μg/g^0.00057μg/g;检测仪器精密度良好,RSD均小于5%;检测方法重现性好,RSD均小于8%;回收率范围在94.91~105.09%。参考《中国药典》和《药用植物及制剂外经贸绿色行业标准》收载的品种项下“农药残留量”部分检查限度,50批中药材检出含有机氯农药检出率占74%,但含量均较低,其中总六六、总滴滴涕和五氯硝基苯超标率分别为16%、12%和4%,50批中药材整体合格率达68%,整体符合要求。结论:气相色谱检测法简便快捷、分离效果好,能广泛用于中药材有机氯农药残留的检测。

In order to provide experimental data for the development and safety control of Chinese herbal medicines,in this study,we determined the content of nine kinds of organochlorine pesticide residues(α-BHC,β-BHC,γ-BHC,δ-BHC,p,p′-DDE,p,p′-DDD,o,p′-DDT,p,p′-DDT,PCNB)in five kinds of Chinese herbal medicines from Guizhou.The samples were ultrasonically extracted with acetone,dichloromethane and petroleum ether.The gas chromatographic-electron capture detection(GC-ECD)Rtx-1701 elastic quartz capillary column(0.25 mm×30 mm×0.25μm)was used for splitless injection.Inlet temperature was 230℃,and detector temperature was 300℃.The temperature rising program was as follows:initial temperature was 100℃,rose to 220℃at 10℃/min,then rose to 250℃at 8℃/min,remaining for 10 min.The content was calculated by external standard method,and the data were statistically analyzed using SPSS 22.0 software.The results showed that,the linear relationship of the nine organochlorines was good,and the correlation coefficient was greater than 0.995.The minimum detection limit was between 0.00012μg/g and 0.00057μg/g.The precision of the detection instruments was good,the RSD was less than 5%.The detection method was reproducible,with the RSD less than 8%.The recovery rate was within the range of 94.91%to 105.09%.The detection rate of organochlorine pesticides in 50 batches of Chinese herbal medicines was 74%,and the excess rate of total HCH,total DDT and PCNB was 16%,12%and 4%respectively.The overall qualified rate of the 50 batches of Chinese herbal medicines reached 68%.In conclusion,this method is simple,rapid,and has good separation effect,and can be widely used in the detection of organochlorine pesticide residues in Chinese herbal medicines.