Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/90554
標題: Temperature controlled liquid phase microextraction in-situ derivatization for determination of estrogens in water by gas chromatography-tandem mass spectrometry
溫度控制液相微萃取即時衍生化結合氣相層析串聯質譜術偵測水中雌激素化合物之研究
作者: 陳顗羽
Yi-Yu Chen
關鍵字: no
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摘要: This study proposed a novel analytical method, temperature-controlled liquid phase microextraction in-situ derivatization combined with gas chromatography-tandem mass spectrometry for determination of trace estrogens in water samples. In optimum conditions, the octanol was utilized as extraction solvent and liquid membrane supported. An aliquot of 11.25 mL water sample (pH 6) containing 5% sodium chloride was mixed with 3.75 mL of 10 μg/mL dansyl chloride derivatization agent. After derivatization for 15 min at 60°C water bath, the derivatives was extracted by liquid phase microextraction with octanol then the extractant was analyzed by GC-MS/MS. The linearity of the proposed method ranged from 0.05 to 50 ng/mL and the coefficients of determination were above 0.9940. The limits of detection (LODs) of six estrogens studied were between 0.3 to 1.1 ng/mL. The intra-day and inter-day precisions ranged from 1.2 to 10.8% and 2.9 to 17.6%, respectively. The recovery of the presented method was between 84.9 and 107.8%. The results demonstrate the adequacy of the presented method for successful determination of trace estrogens in wastewater.
本研究開發以溫度控制液相微萃取 (liquid phase microextriction) 即時衍生化之前處理方式結合氣相層析串聯質譜術之分析,偵測水中六種微量雌激素化合物,包含雌酮、17α-雌二醇、17α-乙炔基雌脂二醇、美雌醇、二乙基己烯雌酚、雙烯雌酚。實驗結果顯示,在溫度控制液相微萃取即時衍生化前處理方法中,添加 5% 氯化鈉於水中,調整水樣為 pH6 和以 10 μg/mL 丹磺醯氯為衍生化試劑且以 3:1(v:v)的比例混合後置於 15 mL 樣品瓶中,將注滿 octanol 之中空纖維放入水樣中,在 60°C 水浴下,加熱衍生萃取 15 分鐘,再利用注射針取出中空纖維內之octanol直接以氣相層析串聯質譜儀進行分析。在最佳萃取與分析條件下分析水樣中六種雌激素之線性範圍介於 0.05 至 50 ng/mL 之間,線性相關係數皆在 0.9940 以上,方法偵測極限介於 0.3 至 1.1 pg/mL 之間。所開發分析方法之同日內精密度與異日內精密度相對標準偏差分別介於 1.2 至 10.8% 之間與 2.9 至 17.6% 之間, 回收率介於 84.9 至 107.8% 之間。應用所開發的方法於河川水、湖水、魚塭水、養豬廢水等各式廢水中微量雌激素之檢測,實驗結果顯示並未測出含有雌激素。本研究方法開發同時進行衍生化及萃取,不但可縮短樣品前處理時間且具高萃取效率以及選擇性,可做為水中微量雌激素之檢測參考。
URI: http://hdl.handle.net/11455/90554
文章公開時間: 10000-01-01
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