GC法检测72种中药饮片有机氯农药残留量

Determination of Organochlorine Pesticide Residues in 72 Chinese Herbal Medicine Tablets by GC

目的:建立检测多种中药饮片有机氯农药残留量的方法。方法:采用气相色谱法。色谱柱为Agilent HP-5弹性石英毛细管柱,检测器为^(63)Ni源电子捕获检测器,进样口温度为250℃,检测器温度为300℃,程序升温,载气为高纯氮,载气流速为1 ml/min,进样量为5μl,不分流进样。结果:α-BHC、β-BHC、γ-BHC、δ-BHC、PP′-DDE、OP′-DDT、PP′-DDD、PP′-DDT检测质量浓度线性范围均为0.01~0.20μg/ml(r分别为0.999 5、0.996 4、0.999 6、0.993 7、0.999 3、0.999 7、0.999 1、0.998 3);定量限分别为0.015、0.02、0.01、0.02、0.01、0.01、0.02、0.62μg/ml;精密度、稳定性、重复性试验的RSD<3.0%;加样回收率为71.2%~109.2%(RSD为4.2%~9.8%,n=9)。72种中药饮片有机氯农药残留总体检出率为66.7%,总体符合标准率为87.5%。结论:该方法操作简便,精密度、稳定性、重复性好,可用于多种中药饮片有机氯农药残留量的检测。

OBJECTIVE： To establish a method for the detecting of organochlorine pesticide residues in 72 Chinese herbal medicine tablets. METHODS： The column was Agilent HP-5 elastic quartz capillary column, detector was 83Ni source electron capture detector, the inlet temperature was 250℃ and the detector temperature was 300℃, temperature programmed, carrier gas was high-purity nitrogen, flow rate of carrier gas was 1 ml/min, and the injection volume was 5 μl, splitless injection. RESULTS：The linear range were 0.01-0.20 5μg/ml for a-BHC-β1-BHC-,7-BHC,5-BHC, PP＇ -DDE、OP＇ -DDT、PP＇ -DDD、PP＇ -DDT（r were 0.999 5, 0.996 4,0.999 6,0.993 7,0.999 3,0.999 7,0.999 1,0.998 3） ;Limit of quantitation were 0.015,0.02,0.01,0.02,0.01,0.01,0.02,0.62 μg/ml; RSDs of precision, stability and reproducibility tests were lower than 3.0% ; recovery was 71.2% -109.2% , RSD was 4.2%-9.8% （n=9）. The overall detection rate of the organochlorine pesticides was 66.7%, and the overall compliance rate was 87.5%. CONCLUSIONS：The method is simple with good precision, stability and reproducibility, and can be used for the detection of organochlorine pesticide residues in Chinese herbal medicine tablets.