2011-01-012024-05-13https://scholars.lib.ntu.edu.tw/handle/123456789/650240摘要:殺蟲劑、殺菌劑、除草劑三者為國內農藥使用之主要種類。本計畫於100年度(第一年)依據行政院農業委員會劇毒農藥資料以及其他風險與毒性評估之文獻,先進行50種殺蟲劑之分析方法開發與環境水體調查,包括30種有機磷,13種氨基甲酸鹽類,與7種合成除蟲菊精。101年度則將針對100年度所蒐集之資料加以評估,加入重要之殺菌劑與除草劑,並補充重要之殺蟲劑活性成分,建議至少100種農藥發展分析方法之優先順序。在分析方法開發方面,現有水體中多重殘留農藥殘留之分析文獻有許多使用Oasis HLB cartridges進行固相萃取;本研究將開發以Atlantic HLB disk(47 mm)固相萃取圓盤搭配SPE-DEX 4790全自動固相萃取系統萃取水樣,並以極致液相層析儀(ultra-performance liquid chromatography, UPLC)搭配串聯式質譜儀以電灑游離(ESI)方式分析上述50種農藥之分析方法。儀器分析預計將分別使用Phenomenex Kinetex PFP(50 × 2.1 mm, 2.6 μm)分析正電荷待測物,Supelco Ascentis Express C18 (50 × 2.1 mm, 2.7 μm)分析負電荷待測物。正、負電荷使用層析動相分別為甲醇/5mM ammonium acetate(pH 6.25)及甲醇/10 mM N-methylmorpholine(pH 9.6),流速皆為0.5 mL/min。此兩種超高效能層析管柱可運用於一般傳統之液相層析儀。為配合委託單位技術轉移之要求,本計畫亦會提供與委託單位同型之串聯式質譜儀操作參數。本年度預計之採樣地點為翡翠水庫、台北長興淨水廠與內湖生活污水處理廠、以及雲嘉南主要河川北港溪(中度到嚴重污染)、八掌溪(稍受污染到中度污染)、及鹽水溪(稍受污染到嚴重污染)之重要支流以及其本流,共計24件實際水樣,以驗證分析方法之適用性,並提出調查分析報告,瞭解50種農藥於該類水體的殘留。<br> Abstract: Insecticides, bactericides and herbicides are the primary pesticides used in Taiwan. According to the information of toxicities and potential health and ecological risks, this project will pick up 50 important pesticides at the first year (2011), including 30 organophosphates, 13 carbamates, and 7 pyrethroides, and will develop and validate an analytical method for water matrixes. Based on the further information that will be gather this year, we will re-evaluate the significance of the 50 pesticides, select critical bactericides and herbicides, and add them into the analyte list for method development in the next year. Most of the existing methods extract pesticides using Oasis HLB cartridges; our study will use Atlantic HLB disks for the solid-phase extraction with SPE-DEX 4790 automatic extractors, and analyze the pesticides with ultra-high performance liquid chromatography coupled with tandem mass spectrometry and electrospray ionization. The separation will be performed on Phenomenex Kinetex PFP column and Supelco Ascentis Express C18 column for positive and negative ions, respectively. Because of much lower back pressure comparing sub-2 μm columns, these two fused-core columns can be used on traditional HPLC instruments. To facilitate the transfer of the new analytical method to the client, we will also optimize the parameters of the same mass spectrometer that uses by the client (the NIEA). Furthermore, to demonstrate the capability of the new method, we will analyze real samples from a reservoir, a drinking water treatment plant, a sewage treatment plant, and surface water from three rivers in agricultural areas, in the total of 24 samples.固相萃取液相層析/串聯式質譜儀農藥有機磷氨基甲酸鹽除蟲菊電灑游離熔融核solid-phase extractionUHPLC/MS/MSpesticidesorganophosphatescarbamatespyrethroidselectrospray ionizationfused-coreMethod development of trace analysis on organics in water