Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/16470
DC FieldValueLanguage
dc.contributor李茂榮zh_TW
dc.contributor謝嘉峰zh_TW
dc.contributor楊慶成zh_TW
dc.contributor陳甫州zh_TW
dc.contributor.advisor鄭政峯zh_TW
dc.contributor.author黃秀華zh_TW
dc.contributor.authorHuang, shiu-huaen_US
dc.contributor.other中興大學zh_TW
dc.date2008zh_TW
dc.date.accessioned2014-06-06T06:55:29Z-
dc.date.available2014-06-06T06:55:29Z-
dc.identifierU0005-1408200617151000zh_TW
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dc.identifier.urihttp://hdl.handle.net/11455/16470-
dc.description.abstract有機氯農藥(Organochlorine Pesticides, OCPs)為揮發性低、不易分解的疏水性物質,雖已停用二十餘年,但由於此種化合物在環境中不易分解、殘留時間長以及對生物具高度累積性與致癌性,在環境中的殘留量仍可能對生態與人體健康產生影響。故建立一套靈敏度高之有機氯農藥殘留的檢測分析方法十分重要。 本研究以微波輔助頂空中空纖維液相微萃取技術(microwave assisted headspace/ hollow fiber- liquid phase microextraction;MA-HS/HF-LPME)結合氣相層析串聯質譜術分析環境水體中之有機氯農藥。研究結果顯示以MA-HS/HF-LPME方法分析環境水體中有機氯的最佳參數為:微波功率277瓦特,冷凝水溫度25℃,中空纖維管長度使用1.5cm,微波照射時間22.5分鐘,正辛醇為萃取溶劑,不調整pH值,以0.2M硫酸銨溶液作為萃取液。以串聯質譜儀最佳分析條件進行有機氯農藥分析,其線性範圍除α、β-Endosulfan及Endosulfan-sulfate為50至1000μg/l外,其餘農藥皆為2.5至100μg/l之間;檢量線之R2值皆於0.9967以上;而最低偵測極限則可達0.2~2 μg/l (安殺番為18 ~41μg/l);均在公告之檢測範圍之內。 傳統檢測有機氯農藥殘留方法都需要使用大量有機溶劑來進行萃取及濃縮的動作,過程繁瑣又冗長並對環境造成危害;而利用本研究之方法可大大縮短傳統萃取所需之時間並且是一種操作簡便、價格低廉、使用少量有機溶劑(3μl)之新方法;偵檢器部分使用氣相層析串聯質譜儀,利用提高訊號雜訊比(S/N ratio)來增加靈敏度使基質干擾降低,成功達到偵測水中有機氯農藥殘留之分析的目的。zh_TW
dc.description.abstractHydrophobic Organochlorine Pesticides (OCPs) had been used widely in Taiwan. But, the OCPs were toxic and easily accumulated in biology. Althoughs, the government announced to forbid utilizing many kinds of OCPs in 1971. The residues of OCPs in the surrounding could still damage the ecology and human being. Thus, it is important to develop a set of sensitive identification method to determine the residues of OCPs. In this study, the microwave assisted-headspace/hollow fiber-liquid phase microextraction (MA-HS/HF-LPME) combined with gas chromatography/ tandem mass spectrometer (GC/MS/MS) was investigated to determine the OCPs residues in surface waters. Water sample solution was accelerated heating by microwave irradiation, and analytes were sampled onto the probe of the hollow fiber supported liquid phase microextraction in a controlled temperature headspace prior to GC/MS/MS analysis. Results indicated that the optimal sampling conditions as with the probe of 3μl 1-octanol in 1.5cm hollow fiber to collect analytes at 25℃ under microwave irradiation of 10 ml sample solution (with 0.2M ammonium sulfate as matrix) at 277 watts for 22.5min. Under the optimal condition, the detection were linear with correction coefficients (R2)>0.9967 in the concentration of 50~100μg/l for α,β-Endosulfan and Endosulfan-sulfate, and is at 2.5~100μg/l for other OCP pesticides. The detection limits varied from 0.2~2μg/l except for Endosulfans in 18~41μg/l. All results mentioned above are met for the requirement as a method for pronounced standards. For the residue of OCPs, the common analytical approach, following the large amount of organic solvent available to extract and concentrate, is complicate and time-consuming. Besides, the used organic solvent is harmful to our environment as well. Thus, the proposed method provides a very simple, low cost, use trace organic solvent (~3μl) in the experiment. Moreover, the detector with GC/MS/MS could increase S/N ratio and improve the sensitivity to reduce the interference of matrix. Eventually, this method, successful to analyze the residue of OCPs in water, is also more easily operative and cheaper than before.en_US
dc.description.tableofcontents摘 要 i Abstract ii 目 錄 iii 圖目錄 vi 第一章、 緒論 1 一、有機氯農藥基本資料 1 二、文獻探討 5 三、前處理技術 7 (一) 液相-液相萃取法 7 (二) 索式萃取方法 8 (三) 液相微萃取法 9 1. 單滴微萃取法 12 2. 液液液微萃取法 14 3. 中空纖維液相微萃取法 14 (四) 頂空間法 16 (五) 頂空中空纖維液相微萃取法 16 (六) 影響HS/HF-LPME萃取效率的實驗參數 18 1. 中空纖維的選擇 18 2. 萃取溶劑的選擇 18 3. 樣品的攪拌 18 4. 樣品溶液與萃取溶液的體積 18 5. 萃取時間 19 6. pH值的調整 19 7. 鹽類的添加 19 (七) LPME的應用 19 四、微波概述與其在化學上之應用 21 (一) 離子傳導 24 (二) 偶極轉動 24 (三) 微波樣品量對加熱的影響 27 (四) 微波加熱方式和傳統加熱方式的比較 27 (五) 微波爐基本結構與功能 29 (六) 微波源功率的輸出與計算 29 (七) 微波使用注意事項及微波安全系統的評估 30 五、質譜儀儀器原理 31 (一) 串聯質譜儀 31 1. 子離子掃描 32 2. 母離子掃描 32 3. 中性丟失掃描 32 4. 選擇反應偵測 32 (二) 離子源 32 (三) 質量分析器 33 六、目的 35 第二章、試驗材料及研究方法 37 一、藥品、器材及儀器設備 37 (一) 藥品 37 (二) 器材及儀器設備 38 二、藥品配製 39 三、玻璃器皿的矽烷化 42 四、氣相層析質譜儀條件之設定 42 五、MA-HS/HF-LPME裝置之建立 43 六、實驗步驟及條件探討 45 (一) 萃取中空纖維管的選擇 45 (二) 注射針與中空纖維管之組合及萃取步驟 45 (三) 微波功率之探討 47 (四) 冷凝水溫度的探討 47 (五) 有機溶劑的選擇 47 (六) 中空纖維管長度的選擇 47 (七) 微波照射時間的探討 47 (八) 萃取液pH值影響的探討 47 (九) 鹽類添加的探討 48 (十) 水中OCPs濃度範圍、校正曲線方程式、相關係數及偵測極限 48 (十一) 精密度的探討 49 七、真實樣品的測定 49 第三章、結果與討論 50 一、氣相層析與分離管柱之選擇 50 二、串聯質譜儀條件最佳化探討 50 三、MA-HF/HS-LPME之最佳化條件探討 73 (一) 微波照射最佳化功率之選擇 73 (三) 萃取溶劑的選擇 77 (四) 中空纖維管長度的選擇 80 (五) 微波照射時間的選擇 82 (六) 萃取液pH的影響 82 (七) 鹽析效應的探討 85 1. 鹽類添加的種類 85 2. 鹽類添加之濃度 85 四、方法可行性之評估 88 (一) 校正曲線及偵測極限 88 (二) 精密度試驗 92 (三) 濃縮倍率 92 (四) 真實樣品之分析 92 第四章、結論 97 第五章、參考文獻 98zh_TW
dc.language.isoen_USzh_TW
dc.publisher化學系所zh_TW
dc.subject有機氯農藥zh_TW
dc.subjectOrganochlorine Pesticides (OCPs)en_US
dc.subject微波輔助zh_TW
dc.subject中空纖維管zh_TW
dc.subject液相微萃取zh_TW
dc.subject氣相層析串聯質譜zh_TW
dc.subjectHollow Fiber (HF)en_US
dc.subjectMicrowave Assisteden_US
dc.subjectLiquid Phase Microextraction (LPME)en_US
dc.subjectGas Chromatography/Tandem Mass Spectrometer (GC/MS/MS)en_US
dc.title以微波輔助頂空中空纖維液相微萃取技術結合氣相層析串聯質譜儀偵測水中有機氯農藥殘留zh_TW
dc.titleDetermination of organochlorine pesticides in water by microwave assisted-headspace/hollow fiber liquid-phase microextraction/ gas chromatography/ tandem mass spectrometeren_US
dc.typeThesis and Dissertationzh_TW
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