摘要
目的:建立同时测定新鲜食用菌中的24种农药残留的气相色谱—串联质谱法。方法:样品匀浆后,加入水、乙腈、盐,水平振摇提取,高速离心后去上清液氮气浓缩,乙酸乙酯定容,GC-MS/MS测定。使用电子轰击离子源(EI)进行电离,多反应监测(MRM)模式对目标物碎片进行采集,内标法定量分析。结果:24种农药的内标曲线在一定质量浓度范围内线性良好,相关系数R 2均在0.9986以上,方法检出限(LOD)为2.0~3.0μg/kg,方法定量限(LOQ)为5.0~10.0μg/kg。在1,2,5倍定量限加标水平下,24种农药加标回收率为76.4%~101.0%,相对标准偏差(RSD)为1.79%~8.98%。结论:该方法具有操作简单、快捷、回收率好、灵敏度高、重现性好等优点,适用于新鲜食用菌中24种农药残留的测定。
Objective:A gas chromatography-tandem mass spectrometry method was established for the simultaneous determination of 24 pesticide residues in fresh edible fungi.Methods:Samples were homogenized and then shaken horizontally for extraction with water,acetonitrile and salt.After high-speed centrifugation,the supernatant was removed and concentrated with nitrogen then reconstituted with ethyl acetate and finally determined by GC-MS/MS.Electron impact ionization(EI)was used for ionization,multiple reaction monitoring(MRM)mode was used to collect target fragments by multiple reaction monitoring(MRM)mode and internal standard method was used for quantitative analysis.Results:24 pesticides showed good linearities in their respective concentration ranges with correlation coefficient(R 2)that were both greater than 0.9986.The limit of detection(LOD)and quantification(LOQ)of the method were in the ranges of 2.0~3.0μg/kg and 5.0~10.0μg/kg,respectively.Average recovery rates of 24 pesticides ranged from 76.4%to 101%with the relative standard deviation(RSD)being 1.79%to 8.98%.Conclusion:The method was simple to operate,rapid,good recovery,high sensitivity and good reproducibility and suitable for the determination of 24 pesticide residues in fresh edible fungi.
作者
沈霞
SHEN Xia(Jiaying University,Meizhou,Guangdong 514087,China)
出处
《食品与机械》
CSCD
北大核心
2023年第3期38-43,225,共7页
Food and Machinery
基金
梅州市科技计划项目(编号:2013B17)
广东省重点领域研发计划项目(编号:2019B020211001)。
关键词
分散固相萃取
气相色谱—串联质谱法
食用菌
农药残留
dispersive solid phase extraction
gas chromatography-tandem mass spectrometry
edible fungi
pesticide residues