農產品中西脫蟎及亞烈寧殘留量檢驗方法之探討   全文下載

Determination of Benzoximate and Allethrin Residues in Crops

本研究利用高效液相層析法及氣相層析法分別檢驗農產品中殺?劑西脫?（benzoximate）及殺蟲劑亞烈寧（allethrin）之殘留量。西脫?之檢驗先以甲醇自作物中抽出，再以二氯甲烷萃取，經減壓濃縮，淨化，定容後，以高效液相層析儀配合Lichrospher RP-18層析管及UV檢出器在235nm波長下可得較佳之偵測。亞烈寧之檢驗則是以丙酮：石油醚（1：2）溶液自作物中抽出，再以2%食鹽水溶液洗雜質，有機層經減壓濃縮，定容後，所得檢液以氣相層析儀配合DB-608毛細層析管柱及ECD檢出器偵測之較佳。甜橙檢體中添加西脫?1、2、3ppm檢體濃度之平均回收率為92.4~94.9%，變異係數1.5~5.1%，最低檢出限量為0.05ppm。而添加亞烈寧於金針菇中1.5、3.0、4.5ppm濃度之平均回收率為90.5~91.0%，變異係數1.5~1.6%，最低檢出限量為0.05ppm。本計畫於民國八十六年二月至五月間於台北市傳統市場及生鮮超市分別抽驗柑桔類檢體及蕈菜類檢體各10件，依所建立的方法檢測，結果柑桔類檢體均未檢出西脫?，而蕈菜類檢體則有2件檢出亞烈寧，檢出量為0.09及0.06 ppm。

High performance liquid chromatography (HPLC) and gas chromatography (GC) were developed to determine benzoximate and allethrin in crops. A residue of benzoximate was extracted with methanol/water solution from citrus fruits and partitioned into dichloromethane, which was then concentrated under reduced pressure, purified with a Sep-Pak Florisil cartridge, and finally determined by HPLC at UV 235 nm using a Lichrospher PR-18 column. A residue of allethrin was extracted with acetone-petroleum ether (1:2) from mushrooms. The extract was then washed with 2% aqueous NaCI, evaporated to dryness under reduced pressure, and reconstituted to volume prior to GC-ECD (electron capture detector) analysis. Recovery studies for benzoximate and allethrin were performed at 1~3 ppm and 1.5~4.5 ppm fortification levels, respectively. Average recoveries were 92.4-94.9% for benzoximate and 90.5~91.0% for allethrin. Coefficients of variation of which were 1.5~5.1 %, and 1.5~1.6%, respectively. The detection limits of both benzoximate and allethrin were 0.05 ppm. When 10 citrus fruits and 10 mushrooms, which were purchased from traditional markets and supermarkets in Taipei between February and May of 1997, were analyzed, no benzoximate was detected in citrus fruits, while 2 mushroom samples contained 0.09 and 0.06 ppm allethrin were detected. 本研究利用高效液相層析法及氣相層析法分別檢驗農產品中殺蟎劑西脫蟎（benzoximate）及殺蟲劑亞烈寧（allethrin）之殘留量。西脫蟎之檢驗先以甲醇自作物中抽出，再以二氯甲烷萃取，經減壓濃縮，淨化，定容後，以高效液相層析儀配合Lichrospher RP-18層析管及UV檢出器在235nm波長下可得較佳之偵測。亞烈寧之檢驗則是以丙酮：石油醚（1 : 2）溶液自作物中抽出，再以2%食鹽水溶液洗雜質，有機層經減壓濃縮，定容後，所得檢液以氣相層析儀配合DB-608毛細層析管柱及ECD檢出器偵測之較佳。甜橙檢體中添加西脫蟎1、2、3ppm檢體濃度之平均回收率為92.4～94.9%，變異係數1.5～5.1%，最低檢出限量為0.05ppm。而添加亞烈寧於金針菇中1.5、3.0、4.5ppm濃度之平均回收率為90.5～91.0%，變異係數1.5～1.6%，最低檢出限量為0.05ppm。本計畫於民國八十六年二月至五月間於台北市傳統市場及生鮮超市分別抽驗柑桔類檢體及蕈菜類檢體各10件，依所建立的方法檢測，結果柑桔類檢體均未檢出西脫蟎，而蕈菜類檢體則有2件檢出亞烈寧，檢出量為0.09及0.06 ppm。