利用串聯式固相萃取技術檢測水產品中多種農藥殘留   全文下載

Multiresidue Determination of Pesticide in Fishery Products by A Tandem Solid-Phase Extraction Technique

本研究建立利用串聯式固相萃取（tandem solid phase extraction）技術，自水產品（包括貝類、甲殼類、魚類及頭足類）中同時萃取4類主要農藥，包括胺基甲酸鹽（carbamate）、有機氯（organochlorine）、有機磷（organophosphate）及合成除蟲菊（synthetic pyrethroid）類農藥，並完成淨化步驟的方法，以利水產品中農藥殘留檢測的工作。在此方法中，甲殼類及魚類樣品直接以乙A進行萃取。除乙A外，貝類樣品須加水及丙酮以調整鹽度並降低極性、頭足類樣品須先加水以利樣品的打碎，兩者在藥劑萃取時並須增加鹽析步驟。各方法的萃取物均利用以C18和aminopropyl固相萃取匣串聯的管柱淨化，乙A為淨化過程中唯一使用的溶劑。殘留藥劑利用氣相層析儀（gas chromatography, GC）附電子捕擭式檢出器（electron capture detector, ECD）及火焰光度檢出器（flame photometric detector, FPD）和液相層析儀（high performance liquid chromatography, HPLC）附螢光檢出器（fluorescence detector）偵測。利用各類水產品中添加不同濃度的標準劑（共4類91種農藥）的回收率評估方法的適用性。試驗結果顯示，除了10個藥劑（包括1-naphthol, 3-hydroxy carbofuran, aldicarb sulfoxide, heptachlor, trifuralin, acephate, dichlorvs, methamidophos, monocrotophos以及omethoate）外，其餘藥劑在供試水產品中的回收率均在60%-120%間且回收率重覆的偏差係數（coefficient variation, CV）均< 20%。本方法有助於水產品中農藥殘留的快速篩檢工作。"

In order to simplify the survey of pesticide (including carbamate, organochlorine, organophosphate and synthetic pyrethroid pesticides) residues in fishery products (including bivalve, crustacean, fish and cuttlefish), multiresidue determination methods were developed through a solid phase extraction (SPE) technique. In the present procedures, samples were extracted with acetonitrile except for bivalve and cuttlefish samples. Mixed solvent of water, acetone and acetonitrile was added to bivalve prior to homogenization, whereas water was needed in cuttlefish samples for blending. For both kinds of sample, an additional procedure of salting-out was needed during extraction. Tandem SPE cartridges of C18 and aminopropyl, using acetonitrile as the only solvent, were used to clean up extracts from either method. A total of 91 pesticides in four major pesticide groups were tested in this study. Gas chromatography (GC, equipped with electron capture detector and flame photometric detector) and high-performance liquid-chromatography (HPLC) equipped with fluorescence detector were used for analysis. The validation of the method was evaluated for each fishery product using samples spiked with all pesticide standards at three concentration levels. The results indicated percentage of recovery ranged from 60% - 120% and coefficients of variation < 20% for all but 10 of the pesticides analyzed (including 1-naphthol, 3-hydroxy carbofuran, aldicarb sulfoxide, heptachlor, trifuralin, acephate, dichlorvs, methamidophos, monocrotophos and omethoate). Residue extraction techniques described in this report are rapid and suitable for screening of pesticide residues in monitoring programs.