| 英文摘要 |
A method using high performance liquid chromatography (HPLC) for the determination of butocarboxim in agricultural products was developed. Butocarboxim was extracted from samples with acetone and the extract solution was concentrated. The residue was dissolved in sodium chloride solution and partitioned with n-hexane. The aqueous phase was collected followed by extracted with dichloromethane, which was then evaporated to a volume of 2 mL prior to passing through an aminopropyl cartridge for sample clean-up. Determination of butocarboxim residue in crops was carried out by HPLC equipped with a post-column derivatization system and a fluorescence detector. HPLC separation was performed on a Lichrospher 60 RP-Select B column eluted with a mobile phase of acetonitrile-water (25:75, v/v). Butocarboxim was hydrolyzed at 90°C under alkaline conditions and subsequently reacted with o-phthaldialdehyde (OPA) / 2-mercaptoethanol reagent via a post-column reactor to generate a fluorophore, which was then detected with a fluorescence detector at Ex 340 nm and Em 455 nm. Average recoveries from radishes and bamboo sprouts, which were spiked with 0.1~0.3 and 0.2 ppm butocarboxim, respectively, were in the range of 81.9~82.6%. The detection limit was 0.05 ppm. No butocarboxim residue was detected in 10 commercial products including radishes, carrots, and bamboo sprouts.
本研究建立了以高效液相層析法檢驗農產品中佈嘉信（butocarboxim）之殘留量。本檢驗法係以丙酮為抽出溶媒，抽出液經減壓濃縮至無溶媒，加入食鹽水，以正己烷振搖去雜質後並以二氯甲烷萃取，經胺基因相萃取匣（aminopropyl cartridge）淨化，以高效液相層析儀配合後置反應裝置及螢光檢測器進行分析。佈嘉信經層析管Lichrospher 60 RP-Select B，移動相乙腈：水 = 25:75 （v／v）分離後，於90°C、鹼性下水解後，和鄰苯二甲醛（o-phthaldialdehyde） ／ 乙硫醇 （2-mercaptoethanol）試劑衍生螢光物質，以螢光檢測器於激發波長340 nm及放射波長455 nm偵測。添加佈嘉信於蘿蔔中0.1～0.3 ppm，平均回收率為81.9～82.6%，添加於麻竹筍中0.2 ppm，平均回收率為82.5%。本檢驗法之最低檢出限量為0.05 ppm。以建立之檢驗方法分析市售檢體，蘿蔔、紅蘿蔔、茭白筍、烏腳綠竹筍及麻竹筍等十件皆未檢出佈嘉信。 |
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