固相萃取-气相色谱法测定蜂蜜中氟胺氰菊酯残留量  

Determination of Fluvalinate Residues in Honey by Solid-Phase Extraction-Gas Chromatography Method

作　　者：孙爱洁 SUN Aijie(Intertek Testing Services Ltd.,Shanghai,Shanghai 200233)

机构地区：[1]上海天祥质量技术服务有限公司,上海200233

出　　处：《食品工业》2024年第11期321-324,共4页The Food Industry

摘　　要：采用正己烷与二氯甲烷(1+1,V/V)混合溶液作为提取液,通过固相萃取-气相色谱-电子捕获法分析蜂蜜中氟胺氰菊酯残留。以有机溶剂提取蜂蜜中氟胺氰菊酯,以弗罗里硅土固相萃取柱净化,通过GC-ECD技术对目标化合物进行分析。采用外标法进行定量分析,线性范围为10~200μg/L,线性相关系数大于0.995,方法检出限为2μg/kg,符合国内外对于蜂蜜中氟胺氰菊酯残留的最大限量规定。当蜂蜜加标氟胺氰菊酯的浓度分别为5,10,50μg/kg时,方法精密度n=7,回收率在79.7%~94.6%之间,标准偏差在1.23%~2.58%之间。该方法简便、快速、灵敏、准确,适用于蜂蜜中氟胺氰菊酯残留分析。In this paper,a mixed solution of n-hexane and dichloromethane(1+1,V/V)was employed as the extraction solvent.The analysis of fluvalinate residues in honey was conducted utilizing a method involving solid-phase extraction coupled with gas chromatography and electron capture detection.The organic solvent facilitated the extraction of fluvalinate from honey,and subsequent purification was achieved through a solid-phase extraction column containing Florisil silica gel.The target compound was quantitatively analyzed using GC-ECD technology.The quantification process adhered to the external standard method,with a linear range spanning from 10μg/L to 200μg/L and a linear correlation coefficient exceeding 0.995.The detection limit of the method was 2μg/kg,which met the maximum limit requirements for fluvalinate residues in honey at home and abroad.When the concentrations of fluvalinate added to honey were 5,10,50μg/kg,respectively,the precision of the method was n=7,and the recovery rate was between 79.7%and 94.6%,with standard deviations ranging from 1.23%to 2.58%.This approach is characterized by its simplicity,rapidity,sensitivity,and accuracy,rendering it is suitable for the analysis of fluvalinate residues in honey.

关 键 词：固相萃取 气相色谱-电子捕获检测 氟胺氰菊酯残留量 测试 

分 类 号：O657.71[理学—分析化学] S896.1[理学—化学]