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

中文关键词:  EMR-Lipid dSPE  气相色谱-串联质谱法  多反应监测  玉米油  农药残留

英文关键词:EMR-Lipid dSPE  gas chromatography-tandem mass spectrometry  multiple reaction monitoring  corn oil  pesticide residues

中文摘要:

      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~ 20 μg/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。

英文摘要:

      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?20 μg/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.