Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/16620
標題: 超臨界流體線上結合固相微萃取與氣相層析質譜於土壤中氯酚檢測之研究
Determination of Chlorophenols in Soil via Supercritical Fluid on Line Solid-Phase Microextraction combined with Gas Chromatography-Mass Spectrometry
作者: 李文心
Li, Wen-Shin
關鍵字: supercritical fluid extraction
超臨界流體萃取
solid-phase microextraction
soil
chlorophenols
固相微萃取
土壤
氯酚
出版社: 化學系所
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摘要: 本研究為探討利用超臨界流體萃取法 ( supercritical fluid extraction, SFE ) 線上結合固相微萃取技術 ( on line solid-phase microextraction ),配合氣相層析質譜儀,測定土壤中微量氯酚。實驗中探討影響萃取土壤中氯酚含量的參數包含:固相微萃取之纖維材質、超臨界流體萃取壓力、溫度及萃取時間。萃取過程中,整個萃取系統不需使用有機溶劑及衍生化步驟,並在定溫密閉空間下,同時進行潔淨步驟 ( cleanup )。實驗結果顯示,利用超臨界萃取法結合線上固相微萃取技術,偵測土壤中氯酚含量的萃取效率,比單一利用超臨界流體萃取或固相微萃取技術之效果更佳。針對2,4-二氯酚、2,4,6-三氯酚、2,3,4,6-四氯酚、五氯酚四種分析物之偵測極限分別為0.7, 0.1, 0.2, 0.6 ng / g,偵測極限皆可至ng / g以下,相對標準偏差則在3 %以下。
This study evaluates supercritical fluid extraction on line solid-phase microextraction ( SFE-SPME ) combined with gas chromatography-mass spectrometry ( GC-MS ) to determine trace chlorophenols in soil samples. The parameters of extraction including fiber of solid-phase microextraction, pressure, temperature of supercritical fluid extraction and extraction time were systematically evaluated. The extract system was in a sealed space at the constant temperature. During extraction procedure, no organic solvent was used and without any derivation. The results showed that determination of chlorophenols in soil samples using SFE combined with SPME is better than that used SFE or SPME only. Detection limits were estimated at the low ng / g levels, for 2,4-dichlorophenol at 0.7 ng / g, for 2,4,6- trichlorophenol at 0.1 ng / g, for 2,3,4,6-tetrachlorophenol at 0.2 ng / g, for pentachlorophenol at 0.6 ng/g. The linearity was obtained with a precision below 3 % R.S.D from 0.5 to 1000 ng / g. The proposed method is fast and highly sensitive for trace chlorophenols detection in a complicated matrix.
URI: http://hdl.handle.net/11455/16620
其他識別: U0005-2207200722504500
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