加速溶剂萃取-GC-MS/MS法测定杨梅种植土壤中5种菊酯类农药

(ASE)-GC-MS/MS Determination of 5 Pyrethroid Pesticides in Arbutus Planting Soil

建立加速溶剂萃取-气相色谱质谱联用技术测定杨梅种植土壤中的氰戊菊酯、联苯菊酯、甲氰菊酯、氯菊酯和溴氰菊酯5种菊酯类残留量的分析方法。采用加速溶剂萃取法对杨梅种植土壤样品进行萃取,乙酸乙酯-正己烷(2︰3, V/V)作为萃取溶剂,弗罗里硅土净化。通过优化质谱分析参数,以保留时间和选择性离子对双定性、峰面积定量,样品于气相色谱质谱仪上以多反应监测模式(MRM)进行分析,外标法定量。结果表明, 5种菊酯类农药在0.02~2.0μg/m L质量浓度范围内线性关系良好,相关系数均大于0.995,检出限均在0.005~0.012 mg/kg之间;5种菊酯类3个不同浓度点(0.05, 0.10和0.50 mg/kg)的农药加标回收率均在78.6%~97.3%之间,精密度测试相对标准偏差(RSD)均小于5%。方法简单、快速,定性及定量结果准确,适用于土壤中菊酯类农药残留的监测。

An analytical method for determination of 5 pyrethroid pesticide fenvalerate, bifentrin, fenpropathrin, permethrin and deltamethrin residuals in waxberry soil by extractor(ASE)-GC-MS/MS was established. The ASE was selected for extracting waxberry soil samples, and ethyl acetate and hexane solution(2︰3, V/V) was selected as extraction solvent. The extracts were cleaned up by alumina neutral forisil. By optimizing mass spectrometry parameters, the retention time and the selective ion pair were used for qualitative and the peak area for quantitative. The samples were analyzed on GC-MS/MS using multiple response monitoring(MRM) mode, external standard method for quantitative. The result showed that the linear relationship among the concentrations of 5 pyrethroids was good in the range of 0.02-2.0 μg/mL;The correlation coefficient was greater than 0.995;The detection limit was between 0.005 and 0.012 mg/kg, the recoveries of three different concentration points(0.05, 0.10 and 0.50 mg/kg) of 5 pyrethroids were between 78.6% and 97.3%, and the RSD of precision test was less than 5%. The method was simple, rapid and accurate with qualitative and quantitative results, and was suitable for the monitoring of pyrethroid residues in soil.