GC法检测72种中药饮片有机氯农药残留量
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篇名: | GC法检测72种中药饮片有机氯农药残留量 |
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摘要: | 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63Ni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5 μl,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0.01~0.20 μg/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、0.62 μg/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。 |
ABSTRACT: | 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 63Ni 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 5 μg/ml for α-BHC、β-BHC、γ-BHC、δ-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. |
期刊: | 2016年第27卷第36期 |
作者: | 刘芳,欧阳慧子,柴士伟,王强,马融 |
AUTHORS: | LIU Fang,OUYANG Huizi,CHAI Shiwei,WANG Qiang,MA Rong |
关键字: | 气相色谱法;有机氯农药残留量;中药饮片 |
KEYWORDS: | Gas chromatography; Organochlorine pesticide residues; Chinese herbal medicine tablet |
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