Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/15799
標題: 微波輔助頂空中空纖維保護液相微萃取結合GC-ECD分析環境中六氯環己烷類農藥之方法開發
Application of microwave assisted headspace-hollow fiber protected liquid phase microextraction in the determination of HCH in environmental samples by GC-ECD
作者: 蔡銘原
TSAI, MING YUAN
關鍵字: Microwave assisted
六氯環己烷
Liquid phase microextraction
Headspace
微波輔助
中空纖維液相微萃取
頂空
出版社: 化學系
摘要: 本研究針對環境土壤及水體中的六氯環己烷類農藥進行檢測;六氯環己烷,1,2,3,4,5,6-hexachlorocyclohexane,又簡稱HCH,屬於有機氯農藥中的一類,共有α、β、γ、δ四種立體異構物,過去曾經被大量使用於農業之殺蟲;研究發現α、β、γ、δ-HCH在環境中皆不易分解,且會對人體健康與環境造成難以彌補的危害,因此對於該類物質之監測不能疏忽。由於現有之HCH傳統檢測方法太過於繁雜、需時冗長且須耗費大量有機溶劑。故本研究以微波輔助頂空中空纖維液相微萃取技術(MAHS/HF-LPME)結合氣相層析儀,分析環境水體以及土壤中殘留之HCH。實驗中,分析物經由微波快速加熱後,隨著水蒸氣汽化至氣相中,藉由擴散作用進入頂空位置的中空纖維管,並為纖維中之萃取溶劑所吸附,同時達到萃取及濃縮的效果。HCH樣品經萃取後,將萃取溶劑抽取定量直接進入氣相層析儀中進行分離並利用電子捕捉偵測器進行偵測。為建立本偵測方法最佳化條件,實驗中分別對影響萃取的因素進行探討,如: 溶劑種類,萃取中空纖維管的位置,微波照射及採樣時間,冷凝系統溫度,微波功率,鹽析效應,水溶液之pH值,腐植酸等影響。在最佳的條件下進行HCH之分析,濃度範圍介於0.1~100μg/l,各化合物偵測極限介於0.032 ~0.37μg/l之間。以此方法應用在偵測真實樣品:於水樣中回收率在88~103%、RSD在5.8~12.6%之間;土壤中回收率介於74~101%、RSD在9.7~17%之間。故以微波輔助頂空中空纖維液相微萃取技術結合氣相層析儀做偵測,為一操作簡便、價格低廉、快速、不受基質干擾、且只需使用極微量有機溶劑之方法,利用本技術來偵測水樣與土壤中殘留之HCH皆有優良的再現性與靈敏度。
The purpose of this study is to detect α、β、γ、δ-hexachlorocyclohexane in environmental water and soil by developing the technique of sample pretreatment, microwave assisted headspace hollow fiber liquid-phase microextraction (MAHS/HF-LPME). The analytes in aqueous matrix are extracted to organic solvent in the fiber of liquid-phase microextraction in the headspace with the aid of microwave irradiation; thus, the analytes in soil matrix were firstly extracted into the aqueous solution and then followed the same procedures in aqueous matrix. After the compounds were collected, the extract was injected in GC injection port and analyzed by GC/ECD. Parameters affecting the extraction efficiency such as selection of solvent, cloud vaptor point, pH in the solution (slurry), addition of salt to sample solution, the humic acid content in the soil, the power and irradiation time of microwave as well as the time of extraction were investigated .The result showed that the optimum extraction efficiency of HCH in aqueous (soil) matrix was obtained by irradiation of sample solution at pH 2 with irradiation power 167 Watt for 6 min. The detection limits varied from 0.032 to 0.371μg/l. The MAHS/HF-LPME method applied to detect the HCH in real water and soil sample and the recovery is between 74%~102 % . The proposed method is a simple, fast, and trace organic solvent procedure for determing HCHs from complicated sample matrix.
URI: http://hdl.handle.net/11455/15799
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