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目的建立一种超声波辅助提取-固相微萃取-气相色谱(UAE-SPME-GC)方法,对13种贵州苗药中10种有机磷类及拟除虫菊酯类农药残留情况快速检测。方法以金银花作为优化对象,样品经有机溶剂超声提取,直接固相微萃取富集,气相色谱-电子捕获检测器进样检测。结果在优化条件下,7种有机磷类农药在5~500μg/L、3种拟除虫菊酯类农药在2.5~250μg/L内线性关系良好,方法回收率为85.6%~112.7%之间,相对标准偏差(RSD)为3.2%~9.8%,检出限为0.02~0.33μg/L。结论 UAE-SPME-GC方法通过直接富集与进样,无需进行净化处理大大减少了传统中药样品前处理的繁琐步骤,能同时对中药材中10种有机磷类及拟除虫菊酯类农药残留量进行测定,是一种简便、环保、快速的分析方法。
OBJECTIVE To establish a method of ultrasonographic assisted extraction-solid phase microextraction-gas chromatography (UAE-SPME-GC) for the rapid detection of 10 organophosphate and pyrethroid pesticide residues in 13 Guizhou Miao medicines. Methods The honeysuckle was used as the optimization object. The samples were extracted by organic solvent, solid-phase microextraction and gas chromatography-electron capture detector. Results Under the optimized conditions, the linear relationship of the seven organophosphate pesticides was between 5 and 500 μg / L and the three pyrethroid pesticides were between 2.5 and 250 μg / L. The recoveries were between 85.6% and 112.7% The standard deviation (RSD) ranged from 3.2% to 9.8% with a detection limit of 0.02 to 0.33 μg / L. Conclusion The method of UAE-SPME-GC can greatly reduce the tedious steps of pretreatment of traditional Chinese medicine samples by direct enrichment and injection without purification, and can simultaneously detect 10 kinds of organophosphorus and pyrethroid pesticide residues in Chinese herbal medicines To determine, is a simple, environmentally friendly and rapid method of analysis.