气相色谱-质谱/负化学源法同时检测芝麻调和油中9种拟菊酯农药  

Simultaneous determination of nine kinds of pyrethroids residues in sesame blend oil by gas chromatography- mass spectrometry with negative chemical ionization

作　　者：魏斌[1] 朱臻怡[1] 张科[1] 魏云计[1] 冯民[1] 王小晋[1] 

机构地区：[1]淮安出入境检验检疫局,江苏淮安223001

出　　处：《中国油脂》2016年第1期88-91,共4页China Oils and Fats

摘　　要：建立了气相色谱-质谱/负化学源法（GC-MS/NCI）同时检测芝麻调和油中9种常见拟菊酯农药残留的快速检测法。芝麻调和油经正己烷溶解、乙腈萃取、C18粉与PSA粉净化后上机,采取选择离子扫描方式检测。结果表明：9种拟菊酯分离良好,未见明显干扰,在标样添加水平为10、20μg/kg和50μg/kg时平均加标回收率在72.0%~115.5%之间,相对标准偏差在2.8%~11.2%之间,除氯菊酯最低定量限（LOQ）为20μg/kg外,其他拟菊酯LOQ都小于5μg/kg。该方法能够满足《日本肯定列表》中对农药限量的要求（≤10μg/kg）。A rapid method for simultaneous determination of nine kinds of common pyrethroids residues in sesame blend oil was established by gas chromatography -mass spectrometry with negative chemical ioni- zation（ GC -MS/NCI）. Sesame blend oil was dissolved in hexane,extracted by acetonitrile and cleaned up by PSA powder and C18 powder, then analyzed by GC -MS/NCI in selected ion monitoring（SIM） mode. The results showed that nine kinds of common pyrethroids were separated well with no obvious interference,the average recoveries and relative standard deviations were 72.0% - 115.5% and 2.8% - 11.2% respectively when the dosages of standard sample were 10,20 μg/kg and 50 μg/kg respectively, and the limits of quantity（LOQ） of all pyrethroids were less than 5μg/kg except permethrin with LOQ 20 μg/kg. The method could meet the pesticide limitation requirement of Positive List System （ ≤ 10 μg/kg）.

关 键 词：气质联用 负化学离子源 拟菊酯 农药检测 芝麻调和油 

分 类 号：TS227[轻工技术与工程—粮食、油脂及植物蛋白工程]