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目的建立黄芪中20种有机氯和拟除虫菊酯类农药的检测方法。方法采用基质固相分散-气相色谱法(MSPD-GC),色谱柱为PH-5石英毛细管柱(30 m×0.25 mm×0.25μm);柱温(程序升温):150℃为起始温度,以5℃/min升至250℃,保持1 min,再以2℃/min升至270℃,保持5 min;进样口温度:230℃;ECD检测器温度:280℃;载气为氮气,测定黄芪中20种有机氯和拟除虫菊酯类农药残留量。结果有机氯和拟除虫菊酯类农药分别在5～500、10～1 000μg/L呈良好线性关系,r为0.997 9～0.999 7。平均回收率(n=9)为83.6%～110.3%(RSD<10%)。结论该方法操作简便快速,可作为中药材中有机氯和拟除虫菊酯类农药残留的测定方法。
Objective To establish a method for the detection of 20 organochlorine and pyrethroid pesticides in Astragalus membranaceus. METHODS: Matrix solid-phase dispersion-gas chromatography (MSPD-GC) was used. The column was PH-5 quartz capillary column (30 m×0.25 mm×0.25 μm); column temperature (programmed temperature): 150°C as the starting temperature. Raise to 250 °C at 5 °C/min, hold for 1 min, then increase to 2 °C/min to 270 °C for 5 min; inlet temperature: 230 °C; ECD detector temperature: 280 °C; carrier gas is nitrogen, Determination of 20 organochlorine and pyrethroid pesticide residues in Astragalus membranaceus. Results There was a good linear relationship between organochlorine and pyrethroid pesticides at 5-500 and 10-1 000 μg/L, respectively. r was 0.997 9-0.999 7. The average recovery rate (n=9) was 83.6% to 110.3% (RSD<10%). Conclusion The method is simple and rapid, and can be used as a method for the determination of organochlorine and pyrethroid pesticide residues in Chinese herbal medicines.