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研究生: 王星翰
Wang, Sing-Han
論文名稱: 纖維電噴灑游離質譜法結合線上微萃取濃縮技術對嘉磷塞的分析與研究
Applications of an on-line microextraction method for use in the analysis of glyphosate based on fiber-spray/mass spectrometry
指導教授: 林震煌
Lin, Cheng-Huang
學位類別: 碩士
Master
系所名稱: 化學系
Department of Chemistry
論文出版年: 2018
畢業學年度: 106
語文別: 中文
論文頁數: 72
中文關鍵詞: 嘉磷塞中空纖維液-液微萃取
英文關鍵詞: glyphosate, hollow fiber, liquid-liquid microextration
DOI URL: http://doi.org/10.6345/THE.NTNU.DC.005.2018.B05
論文種類: 學術論文
相關次數: 點閱:130下載:6
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  • 為了分析嘉磷塞,本研究開發了結合線上微萃取濃縮技術及纖維電噴灑游離質譜法的方法,本研究利用2毫升樣品瓶(儲存樣品溶液)及一小段中空纖維管(用來進行萃取, 3.5公分長, 外徑/內徑, 1.0 mm/0.6 mm)製作裝置,此微萃取裝置可架設於電噴灑游離源與質譜口之間,分析物能利用中空纖維液相微萃取操作過程,從稀的溶液被提取出來,被提取出來的分析物會透過擴散移動到纖維外,濃縮的分析物被蒸發並通過多孔表面逸出,同時間,由電噴灑游離源產生帶電液珠,一旦來自中空纖維表面(大部分為中性)的蒸發物質遇到電噴霧,游離化便會發生。本實驗用於液相微萃取的液膜為體積比octanol:Aliquat 336:dodecane = 0.4:1:8.6,萃取溶液為0.1 M HCL,利用此方法最低偵測極限可以達到1 ng/mL。當使用攪拌子攪拌時,萃取時間可以從60分鐘減少至僅15分鐘。

    For the analysis of glyphosate, a novel method based on the combination of on-line microextraction and fiber-spray/mass spectrometry was developed. A microextraction kit was designed for this purpose, in which a 2 mL sample vial (reservoir for the sample solution) and a piece of a porous polypropylene hollow fiber (for sample extraction; 3.5 cm in length; O.D./I.D., 1.0/0.6 mm, respectively) were used, respectively. The microextraction kit was located between the mass inlet and the ESI needle. Analytes can be extracted from a very dilute solution operating the so-called hollow fiber liquid phase microextraction process, and the resulting extract then moves to the outside portion of the fiber by diffusion. Following this, the concentrated analytes were evaporated and escape through the porous surface. Meanwhile, the electrosprayed/charged droplets are produced from a regular ESI stainless needle. Once the evaporated materials from the surface of the hollow fiber (mostly neutral) meet the electrospray plume, ionization occurs under ambient conditions. In order to process liquid-phase microextraction, the membrane solution (0.2 M Aliquat 336 in dodecane modified with 4% octanol) and an acceptor solution (0.1 M HCl) were used, respectively. Using the setup, it was possible to improve the limit of detection after microextraction by ∼1000-fold. The limit of detection achieved was 1 ng/mL. When a stir bar was used, the extraction time can be shortened from 60 min to only 15 min.

    目次 摘要 I ABSTRACT II 目錄 III 圖目錄 VI 表目錄 IX 第一章 緒論 1 1-1. 研究目的 1 1-2. 研究介紹 2 1-3. 分析物介紹 4 第二章 分析方法及原理 7 2-1. 液-液相微萃取法(LIQUID-LIQUID MICROEXTRACTION, LLME) 7 2-2. 中空纖維液-液相微萃取法基本原理 10 2-3. 液相層析電噴灑串聯式質譜儀(LC/ESI-MS) 12 2-4. 電噴灑游離質譜法的發展演進 13 2-5. 電噴灑離子化原理及機制 21 第三章 儀器、藥品與實驗方法 24 3-1. 中空纖維液-液相微萃取(HOLLOW FIBER/LIQUID-LIQUID MICROEXTRACTION) 24 3-2. 中空纖維液-液相微萃取結合電噴灑游離質譜法 26 3-3. 儀器及周邊設備列表 30 3-4. 藥品列表 32 3-5. 樣品配製 34 第四章 結果與討論 35 4-1. 纖維電噴灑之最佳位置 35 4-2. 萃取嘉磷塞標準品 37 4-3. 萃取市售除草劑(年年春) 40 4-4. 萃取時間對於萃取效率之探討 42 4-5. 磁石攪拌對於萃取效率之探討 44 4-5-1. 磁石轉速探討 44 4-5-1. 磁石攪拌萃取時間探討 46 4-6. 微波對於萃取效率之探討 48 4-7. 其他多孔中空纖維薄膜 50 4-8. 毛筆採樣結合電噴灑質譜法研究 56 4-8-1. 老鼠咖啡因及其代謝物偵測 56 4-8-2. 人類咖啡因及其代謝物偵測 61 第五章 結論 62 參考文獻 63

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