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National Chung Hsing University Institutional Repository - NCHUIR > 理學院 > 化學系所 > 依資料類型分類 > 碩博士論文 >  開發微萃取技術結合質譜術於環境水樣中氯酚與尿液中利尿劑之檢測研究

Please use this identifier to cite or link to this item: http://nchuir.lib.nchu.edu.tw/handle/309270000/152322

標題: 開發微萃取技術結合質譜術於環境水樣中氯酚與尿液中利尿劑之檢測研究
Developments of Microextraction Techniques Combined with Mass Spectrometry for Analysis of Chlorophenols in Aqueous Sample and Diuretics in Urine Sample
作者: 何澤宗
Ho, Tse-Tsung
Contributors: 李茂榮
Maw-Rong Lee
化學系所
關鍵字: 微萃取技術;固相微萃取;液相微萃取;分散式微固相萃取;離子液體;奈米碳管;垃圾場滲出水;尿液;氯酚;利尿劑;氣相層析質譜儀;液相層析串聯質譜儀
microextraction technique;solid-phase microextraction;liquid-phase microextraction;dispersive micro solid phase extraction;ionic liquid;carbon nanotubes;landfill leachate;urine;chlorophenols;diuretics;gas chromatography-mass spectrometry;liquid chromatography-tandem mass spectrometry
日期: 2013
Issue Date: 2013-11-07 13:20:44 (UTC+8)
Publisher: 化學系所
摘要: 本研究開發了新穎的微萃取技術,主要利用離子液體-固相微萃取偵測垃圾場滲出水中氯酚,將合成離子液體 (1-butyl-3-methylimidazolium hexafluorophosphate, [C4MIM][PF6]) 塗覆於市售損壞的固相微萃取纖維基材上,結合氣相層析質譜儀進行脫附與定量分析。實驗室自製的離子液體-固相微萃取沒有殘留記憶效應 (carryover effect) 及可重覆使用 80 次以上。四種氯酚在垃圾場滲出水中調整 pH 值為 2 ,頂空萃取 4分鐘,在氣相層析儀進樣口溫度 240 °C 下,進行脫附 4 分鐘。四種氯酚線性範圍為0.1 到 1000 μg L-1 ,方法確效之回收率超過 87 % ,精密度的相對標準偏差 (RSD) 均小於 5 % 。五氯酚的偵測極限為 0.008 μg L-1 ,偵測垃圾場滲出水真實樣品檢測出2,4,6-三氯酚與五氯酚,濃度分別為 1.1 與 1.4 μg L-1 ,結果顯示離子液體-固相微萃取結合質譜術方法,適合垃圾場滲出水中檢測。
開發奈米碳管固定於中空纖維液相微萃取之的微萃取技術,偵測尿液中八種利尿劑,在此研究中利用奈米碳管當吸附材質在三相系統液相微萃取中萃取尿液中利尿劑,最後使用液相層析串聯質譜儀分析。實驗結果顯示為本實驗採用二階段的萃取,八種利尿劑在尿液中調整 pH 值為 2 ,鹽類添加 5% ,攪拌速度為 1000 rpm ,第一階段在 25 °C 下萃取時間為 30 分鐘,第二階段在 50 °C 下萃取 4分鐘,再取出萃取溶劑進行分析。八種利尿劑線性範圍為 1 到 1000 ng/mL ,偵測極限介於0.09 到 0.51 ng/mL ,方法確效之回收率超過 87 %,精密度小於 6 % 。利用本研究開發之方法應用於真實尿液樣品分析,可成功地偵測尿液中含有微量利尿劑。
另一個所開發微萃取技術主要是利用奈米碳管與正辛醇加入於分散式微固相萃取結合液相層析串聯質譜儀偵測尿液中十四種利尿劑。實驗結果顯示於十四種利尿劑在尿液中調整 pH 值為 4,不加任何鹽類,尿液樣品體積 1 mL,添加10 mg 奈米碳管 / 100 μL 正辛醇溶液,之後置於超音波萃取 90秒後,再利用甲醇溶劑進行脫附 4 分鐘。十四種利尿劑的偵測極限為 0.027 到 0.293 ng mL-1 ,線性範圍為 0.05到 1000ng mL-1 ,方法確效之回收率超過 86 % ,精密度小於 6.6 % 。此開發的微萃取技術應用在真實樣品的偵測上,可成功地測出尿液中含有微量利尿劑 hydrochlorothiazide 濃度為 1.28 ng/mL。結果顯示奈米碳管-分散式微固相萃取結合質譜術偵測尿液中利尿劑是快速、準確及分析成本低。
A new microextraction technique based on ionic liquid solid-phase microextraction (IL-SPME) was developed for determination of trace chlorophenols (CPs) in landfill leachate. The synthesized ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate ([C4MIM][PF6]), was coated onto the spent fiber of SPME for extraction of trace CPs. After extraction, the absorbed analytes were desorbed and quantified using gas chromatography-mass spectrometry (GC/MS). The term of the proposed method is as ionic liquid-coated of solid-phase microextraction combined with gas chromatography-mass spectrometry (IL-SPME-GC/MS). No carryover effect was found, and every laboratory-made ionic liquids-coated-fiber could be used for extraction at least eighty times without degradation of efficiency. The chlorophenols studied were 2,4-dichlorophenol (2,4-DP), 2,4,6-trichlorophenol (2,4,6-TCP), 2,3,4,6-tetrachlorophenol (2,3,4,6-TeCP), and pentachlorophenol (PCP). The best results of chlorophenols analysis were obtained with landfill leachate at pH 2, headspace extraction for 4 minutes, and thermal desorption with the gas chromatograph injector at 240 °C for 4 minutes. Linearity was observed from 0.1 to 1000 μg L-1 with relative standard deviations (RSD) less than 5 % and recoveries were over 87%. The limit of detection (LOD) for pentachlorophenol was 0.008 μg L-1. The proposed method was tested by analyzing landfill leachate. The concentrations of chlorophenols were detected to range from 1.1 to 1.4 μg L-1. The results demonstrate that the IL-SPME-GC/MS method is highly effective in analyzing trace chlorophenols in landfill leachate.
A novel microextraction technique utilizing the adsorptive potential of immobilized multi-walled carbon nanotubes (I-MWCNT) in hollow fiber liquid-phase microextraction (HF-LPME) was developed for the determination of diuretics in urine. In this study, the potential of carbon nanotubes as a sorbent for three-phase liquid-phase microextraction of diuretics from urine samples was evaluated. Analysis was performed using liquid chromatography-tandem mass spectrometry (LC-MS/MS). A novel method was applied to detect acetazolamide (AAA), chlorothiazide (CTA), hydrochlorothiazide (HCT), hydroflumethiazide (HFT), clopamide (CA), trichlormethiazide (TCM), althiazide (AT) and bendroflumethiazide (BFT) in urine. Two-step extractions using different times and temperatures for each step were adopted. An acceptor solution of 10 mM ammonia, with 5% NaCl added to the urine samples, a stir rate of 1000 rpm, a first-step extraction time of 30 minutes at 25°C and a second-step at 50 °C for 4 minutes were found to be optimal. Under the resulting optimal extraction conditions, this method showed good linearity over an analytes concentration range of 1 to 1000 ng/mL, high extraction repeatability with relative standard deviations of less than 6%, and low detection limits (0.09 to 0.51 ng/mL). The application of the methods to the determination of diuretics in real samples was tested by analyzing urine samples of patient.
A novel microextraction technique based on multi-walled carbon nanotubes (MWCNTs) in dispersive micro solid phase extraction (DMSPE) combined with liquid chromatography tandem mass spectrometry detection is developed for determination of diuretics in urine. The diuretics studied are including acetazolamide (AAA), althiazide (AT), bendroflumethiazide (BFT), bumetanide (BT), ethacrynic acid (EAA), furosemide (FUR), hydrochlorothiazide (HCT), Hydroflumethiazide (HFT), indapamide (INA), indomethacin (IND), probenecid (PRO), spironolactone (SP), triamterene (TA), trichlormethiazide (TCM). A extraction solution of 100 μL MWCNTs n-octanol solution (10 mg MWCNTs) added to the urine samples, a ultrasonic extraction time of 90 seconds and a desorption for 4 minutes with methanol were found to be optimal. The results showed low detection limits are obtained from 0.027 to 0.293 ng mL-1 with good linearity (0.05-1000 ng mL-1) and relative standard deviations less than 6.6 %. The proposed method was tested by analyzing real patient urine samples. Hydrochlorothiazide was detected in real urine samples. Results of this study demonstrate the MWCNTs in DMSPE technique is fast, accurate and cost-effective for extraction of trace diuretics in urine samples.
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