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A Multiresidue Method for Determining 136 Pesticides and Metabolites in Fruits and Vegetables: Application of Macroporous Diatomaceous Earth Column

應用多孔性矽藻土管柱於蔬果中農藥多重殘留分析

摘要


本研究開發了一項快速、簡便、可檢測蔬果中136種農藥及代謝物之多重殘留方析方法。應用多孔性矽藻土(macroporous diatomaceous earth, MDE)管柱取代分液漏斗進行液/液分配萃取,可大幅減少有機溶媒之使用量及處理時間,且無檢液乳化問題。歐殺松(acephate)等51種農藥以氣相層析儀配合脈衝式火焰光度檢出器(GC/PFPD)偵測;阿特靈等63種農藥以氣相層析儀配合電子捕獲檢出器(GC/ECD)偵測;得滅克(aldicarb)等20種胺基甲酸鹽類農藥以高效液相層析儀配合螢光檢出器(HPLC/FLD)偵測;貝芬替(carbendazim)及腐絕(thiabendazole)2種benzimidazole農藥以高效液相層析儀配合紫外光檢出器(HPLC/UV)偵測。於作物中外添加0.05~2 ppm農藥,三重複添加回收試驗之結果顯示回收率及再現性皆良好,方法之最低檢出限量介於0.003~0.2 ppm。本研究建立之農藥多重殘留分析檢驗方法可應用於其他農藥或基質之檢測,檢液製備流程簡便且溶媒使用量少,是一個環保而值得推廣之方法,可應用於蔬果等檢體之例行性農藥殘留檢驗工作。

並列摘要


A fast and easy multiresidue method using the macroporous diatomaceous earth (MDE) column for determining 136 pesticide and metabolite residues in fruits and vegetables was developed. The MDE column was used instead of the separation funnel for liquid/liquid partition in sample preparation. Through MDE columns, the preparation of test solution became easier and faster than traditional funnel liquid/liquid partition. The emulsion problem can also be avoided. Fifty one pesticides including acephate were determined by gas chromatography (GC) with a pulsed flame photometric detector (GC/PFPD) and 63 pesticides including aldrin were detected by GC with electron capture detection (GC/ECD). Twenty carbamate peticides and metabolites including aldicarb were determined by high performance liquid chromatography with a post-column derivaization system and a fluorescence detector (HPLC/FLD) and two benzimidazole pesticides including carbendazim and thiabendazole were detected by HPLC with an ultraviolet detector (HPLC/UV). Recovery studies were performed by spiking pesticides (0.05~2.0 ppm) in fruit and vegetable samples, and the triplicate results showed satisfactory recoveries and repeatability. The detection limits ranged from 0.003 to 0.2 ppm. The developed multireside method can be employed to other pesticides or matrices with an easier and less solvent consumption way to prepare sample solution. It is an environment-friendly and useful method for routine pesticide analysis.

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