土壤中6种白蚁防治药物的超高效液相色谱检测方法研究

Analysis of six termite pesticide residues in soil by ultra performance liquid chromatography

目的建立超高效液相色谱法(UPLC)测定土壤中6种白蚁防治药物——吡虫啉、氟虫腈、虫螨腈、毒死蜱、氰戊菊酯、联苯菊酯残留量的分析方法。方法样品用乙腈匀浆提取,经离心、NH2固相萃取小柱净化、浓缩、定容后,采用超高效液相色谱法进行测定,外标法定量。结果所有农药在0.01~5.00 mg/L范围内线性关系均良好,相关系数r2>0.99;所有农药的方法检出限均低于10μg/kg;在0.050 0、0.167和0.500 mg/kg添加水平下,样品平均回收率为83.0%~117.0%,相对标准偏差RSD为2.0%~4.4%。结论本方法简便,重现性良好,可用于土壤中吡虫啉、氟虫腈、虫螨腈、毒死蜱、氰戊菊酯、联苯菊酯6种药剂残留的检测。

Objective To develope a method for the determination of 6 pesticide residues for termite prevention,including imidacloprid,fipronil,chlorfenapyr,chlorpyrifos,fenvalerate and bifenthrin,in soil by ultra performance liquid chromatography（ UPLC）. Methods The pesticide residues in soil samples were extracted with acetonitrile.After centrifugation,the pesticide residues in the super natant were cleaned up by SPE column of NH2. Concentrated to a definite volume,the targeted compounds were analyzed by UPLC and quantified by the external standard method.Results The results indicated the linear correlation coefficients were greater than 0. 99 when the pesticides ranged between 0. 010 0 and 5. 00 mg/L. The detection limits of 6 pesticides were less than 10 μg/kg. The average spiked recoveries at levels of 0. 050,0. 167 and 0. 500 mg/kg were found to be in the range of 83. 0% to 117. 0%,with the relative standard deviations（ RSD） between 2. 0% and 4. 4%. Conclusion This method was suitable for the determination of 6 pesticide residues for termite prevention in soil due to its simplicity and good sensitivity.