UAE-SPME-GC法对13种苗药中有机磷及拟除虫菊酯类农药残留量的同时测定

Simultaneous determination of residual amount of organophosphorus and pyrethroid pesticides in 13 Miao ethnomedicines using UAE-SPME-GC

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 new gas chromatography （GC） method coupled with ultrasound- assisted extraction （UAE） and solid-phase microextraction （ SPME ） for rapid determination of seven kinds of organophosphorus pesticide residues and three kinds of pyrethroid pesticide residues in 13 Miao ethnomedicines produced in Guizhou province. Methods Japanese Honeysuckle Flower （Flos Lonicerae Japonicae, Jinyinhua） was the optimization object. SPME was used directly for enrichment of extracts obtained by ultrasonic-assisted solvent. Then gas chromatography-electron capture detector was used for the determination. Results Under optimum conditions, seven kinds of organophosphorus pesticides showed a good linear relationship at the range from 5 to 500 μg/L, and three kinds of pyrethroid pesti- cides did at the range from 2.5 to 250 μg/L. The recovery was from 85.6 % to 112.7 % with the RSD 3.2% - 9.8%. The limit of detection was from 0.02 to 0.33 μg/L. Conclusion UAE-SPME-GC established is an easy, environmental-friendly and rapid method for simultaneous determination of residual amount of 10 organophosphorus and pyrethroid pesticides in Miao ethomedicines. This method with directly enriching and sampling , was a simplified sample pretreatment procedure without purification process .