EMR-Lipid dSPE结合气相色谱-串联质谱法同时测定玉米油中218种农药残留

Simultaneous determination of 218 kinds of pesticide residues in coin oil by gas chromatography-tandem mass spectrometry combined with EMR-lipid dSPE

目的建立EMR-Lipid dSPE结合气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)同时测定玉米油中218种农药残留的分析方法。方法样品采用乙腈提取并经冷冻离心初次除油后用EMR-Lipid dSPE分散固相萃取净化,气相色谱-质谱联用仪多反应监测(multiple reaction monitoring,MRM)模式检测,采用基质匹配标准溶液内标法定量。结果218种农药在5~200 ng/mL范围内线性关系良好,相关系数均大于0.995,在0.05、0.10、0.50 mg/kg 3个添加水平的回收率为63.3%~119.9%,相对标准偏差(relative standard deviations,RSDs)为0.78%~18.10%,定量限(limits of the quantitation,LOQs)为10~20μg/kg。结论该方法前处理简单、高效,灵敏度、准确度和精密度高,能满足玉米油中218种农药多残留的分析要求。

Objective To establish a method for the simultaneous determination of 218 kinds of pesticide residues in corn oil by EMR-Lipid dSPE combined with gas chromatography-tandem mass spectrometry(GC-MS/MS).Methods The samples were extracted with acetonitrile and degreased by refrigerated centrifugation,and then used EMR-Lipid dSPE purification tube to purify 218 kinds of pesticides.The target compounds were detected using multiple reaction monitoring multiple reaction monitoring(MRM)on GC-MS/MS system and quantified with internal standard method by the matrix match standard solutions.Results Two hundred and eighteen kinds of pesticides had good linear relationships in the range of 5-200 ng/mL,with the correlation coefficients were greater than 0.995.The average recoveries of the 218 kinds of pesticide residues ranged from 63.3%-119.9%at the spiked levels of 0.05,0.10 and 0.50 mg/kg,with the relative standard deviations(RSDs)of 0.78%-18.10%.The limits of the quantitation(LOQs)were 10-20μg/kg.Conclusion This method has the advantages of simple pretreatment,high efficiency,high sensitivity,accuracy and precision,and can meet the requirements for the analysis of 218 kinds of pesticide residues in corn oil.