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目的:建立白芍中20种有机氯和拟除虫菊酯类农药的检测方法。方法:采用中空纤维液相微萃取-气相色谱法,色谱柱为HP-5石英毛细管柱(30m×0.25mm×0.25μm);柱温(程序升温):150℃为起始温度,以5℃.min-1的升温速率升至250℃,保持1min,再以2℃.min-1的升温速率升至270℃,保持5min;进样口温度:230℃;ECD检测器温度:280℃;载气为氮气,测定白芍中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0.4～40μg.L-1和0.8～80μg.L-1范围内呈良好线性关系,r值范围为0.9970～0.9998。平均回收率(n=9)为82.5%～109.2%(RSD<10%)。结论:该方法操作简便快速,灵敏度高,准确度好,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 determination of 20 organochlorine and pyrethroid pesticides in Radix Paeoniae Alba. Methods: Hollow fiber liquid phase microextraction-gas chromatography was used. The column was HP-5 quartz capillary column (30m × 0.25mm × 0.25μm). The column temperature (programmed temperature) was 150 ℃ and the temperature was 5 ℃ .min-1 heating rate was raised to 250 ℃, holding 1min, then 2 ℃ .min-1 heating rate rose to 270 ℃, holding 5min; inlet temperature: 230 ℃; ECD detector temperature: 280 ℃; The carrier gas is nitrogen, and the determination of 20 organochlorine and pyrethroid pesticide residues in Radix Paeoniae Alba was carried out. Results: There was a good linear relationship between organochlorine and pyrethroid pesticides in the range of 0.4 ~ 40μg.L-1 and 0.8 ~ 80μg.L-1, respectively. The range of r value was 0.9970 ~ 0.9998. The average recovery (n = 9) was 82.5% to 109.2% (RSD <10%). Conclusion: The method is simple, rapid, sensitive and accurate. It can be used as a method for determination of organochlorine and pyrethroid pesticide residues in Chinese herbal medicines.