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目的:建立了基于基质分散固相萃取技术的昆明山海棠中氯氰菊酯、溴氰菊酯、三氟氯氰菊酯、氰戊菊酯、甲氰菊酯、敌敌畏、马拉硫磷、对硫磷、乐果、甲拌磷、毒死蜱、甲胺磷、甲基对硫磷等13种农药的多成分残留分析方法。方法:前处理中以乙腈为提取溶剂、采用弗罗里硅土为分散净化剂的固相萃取方法,并利用超高效液相色谱-串联质谱(UPLC-MS/MS)在多反应离子监测模式(MRM)下进行检测,外标法定量。结果:在0.25~250 ng·mL~(-1)添加水平范围内,13种农药的平均回收率为76.2%~105.5%;相对标准偏差(RSD,n=5)为1.1%~13.1%;方法检出限(LOD)在0.02~7.60μg·kg~(-1)范围内;定量限(LOQ)在0.05~25.95μg·kg~(-1)范围内。结论:该方法快速简便、稳定可靠,适用于有昆明山海棠中机磷和拟除虫菊酯类农药残留的检测。
OBJECTIVE: To establish a method for the determination of cypermethrin, deltamethrin, cyhalothrin, fenvalerate, fenvalerate, fenpropathrin, dichlorvos, malathion, parathion, dimethoate , Phorate, chlorpyrifos, methamidophos, methyl parathion and other 13 kinds of pesticides multi-component residue analysis. Methods: Solid phase extraction with Florisil as disperse decontamination agent was used in the pretreatment. Acetonitrile was used as the extraction solvent, and by UPLC-MS / MS, (MRM) under the test, external standard quantitative. Results: The average recoveries of 13 pesticides ranged from 76.2% to 105.5% within the range of 0.25-250 ng · mL -1. The relative standard deviations (RSDs, n = 5) ranged from 1.1% to 13.1%. The limit of detection (LOD) was in the range of 0.02 ~ 7.60μg · kg -1 and the limit of quantification (LOQ) was in the range of 0.05 ~ 25.95μg · kg -1. Conclusion: The method is rapid, simple, stable and reliable. It is suitable for the detection of phosphorus and pyrethroid pesticide residues in Begonia tuberosus.