應用液-液-液微萃取配合高效液相層析儀偵測水中磺胺藥、氯酚化合物、硝基酚化合物與烷基酚化合物

Application of liquid-liquid-liquid microextraction and high performance liquid chromatography for the determination of sulfonamides, chlorophenols, nitrophenols, and alkylphenols in water

林哲毅(Che-Yi Lin)

指導教授 ： 黃賢達

國立清華大學/理學院/化學系/博士(2008年)

摘要

近來利用微萃取技術分析水樣是越來越普遍，微萃取是環境友善、低成本且操作簡易的技術。
在本文中利用一種名為液-液-液微萃取的技術，去分別萃取水中待測的磺胺藥、氯酚化合物、硝基酚化合物與烷基酚化合物。液-液-液微萃取技術是藉由pH值調整使待測物解離或不解離，因而調控待測物的親水性，使待測物能由水樣授予相萃取到有機相，再從有機相萃取至接受相。萃取後在接受相的待測物直接以高效液相層析儀作分析。為了能最佳化實驗條件，將藉由理論模擬來探討哪些參數可以影響萃取效率。實驗中液-液-液微萃取技術被設計為動態的模式以及在非平衡的考量下去萃取水中待測分析物；且在單變法下去操作萃取而確認每一個參數效應後，再指定一組合理參數值作為實驗的參數設定。在所選擇的參數設定下，操作萃取分析而求得相對標準偏差、線性與方法偵測極限，以作為此一技術的成效評估。優越的萃取效率源自於實驗的參數設定是相當接近最佳化的實驗條件。此外，也利用此一技術分析環境水樣來確認實際應用的可行性，操作液-液-液微萃取技術時，水樣的基質效應將造成待測物從授與相經由有機相遷移到接收相的過程會受到干擾，從結果來看，液-液-液微萃取的基質效應是不明顯的。
依實驗所能達到的偵測結果，驗證了此一用來分析水中這些微量待測物的技術是非常有力的。

關鍵字

微萃取

並列摘要

Currently, microextraction is being used more and more for aqueous sample analysis. The microextraction technique is environmentally-friendly, less expensive, and simple to operate. In the study a microextraction technique termed as liquid-liquid-liquid microextraction (LLLME) was implemented to extract sulfonamides, chlorophenols, nitrophenols, and alkylphenols in water. The LLLME technique can control the analytes into uncharged or charged species by pH adjustment, the target compounds were extracted from the donor phase (i.e., a water sample) into the organic phase and then extracted into the acceptor phase (i.e., the extractant). The extracted target analytes in the donor phase were directly separated and quantitated by high performance liquid chromatography (HPLC). To pursue optimum condition in LLLME, extraction parameters dominating extraction efficiency were investigated by theoretical considerations. The LLLME technique under dynamic mode and non-equilibrium consideration was applied for determination of these target analytes in water. The univariant method was conducted to identify extraction parameters for the designation of parameter settings in this dynamic LLLME technique. Relative standard deviation, coefficient of estimation, and detection limit were realized to assess analysis performance under selected parameter settings. The parameter settings of LLLME close to optimization was responsible for an acceptable extraction efficiency. In addition, real field water samples were analysed to demonstrate the practical applicability. The results suggested that matrix effect, interfering in the transport of target compounds from the donor phase through the organic phase and finally into the acceptor phase, was limited. Consequently, the study reachable of the determination confirms LLLME combined with HPLC to be robust to monitoring these target analytes in trace levels.

並列關鍵字

HASH(0x1b3aacf0)

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