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研究生: 吳欣芳
Shin-Fang Wu
論文名稱: 利用無溶劑萃取技術快速測定環境固態樣品中之多環類麝香化合物的研究
Fast Determination of Synthetic Polycyclic Musks in Solid Samples by Solvent Free Techniques
指導教授: 丁望賢
Wang-Hsien Ding
口試委員:
學位類別: 碩士
Master
系所名稱: 理學院 - 化學學系
Department of Chemistry
畢業學年度: 98
語文別: 中文
論文頁數: 103
中文關鍵詞: 氣相層析質譜儀多環類麝香固相微萃取法
外文關鍵詞: Polycyclic Musks, GC-MS, SPME
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  • 從古代開始,香氛就經常被用來增加對於個人的吸引力,而麝香因為在香精工業中被大量使用而佔有一席之地。多環類合成麝香作為天然麝香的平價替代品,在生產製造過程以及一般大眾使用後會隨著污水處理廠處理過後的污水及污泥排放到環境當中,而主要的污染源頭即為這些廢污水以及污泥。
    本篇研究中,利用一步完成的微波輔助頂空固相微萃取裝置搭配氣相層析質譜儀分析廢污泥、沉積物以及牡蠣樣品,方法不僅快速且不須使用有機溶劑。將除水後的固態樣品與20毫升的去離子水混合,以PDMS-DVB的塗附纖維置於樣品頂空後,使用80瓦微波,萃取5分鐘。此方法的偵測極限為0.04至0.1 ng/g,而定量極限為0.1至0.3 ng/g。
    對於這些環境樣品的初步檢測結果顯示,HHCB以及AHTN為最普遍被
    檢測到的兩種多環類麝香化合物,利用標準添加法進行定量分析,待測物的總濃度介於0.3至10.9 ng/g,而再現性的相對標準偏差範圍為4 %至10 %。
    本實驗所開發的微波輔助頂空固相微萃取法,搭配氣相層析質譜儀的選擇離子掃描偵測模式,為一種具有可靠性且靈敏度高的檢測方法,提供了一個方便的檢測技術以檢測環境固態樣品中微量的多環類麝香化合物。


    Fragrances have been used increase attractiveness of persons since ancienttimes. Musk is one of the most important and often used fragrances in perfumery. Synthetic polycyclic musks are inexpensive substitutes for natural musks. Synthetic polycyclic musk compounds enter environment principally through effluents of wastewater treatment plants and waste sludge, and the major source of environmental pollution of synthetic musks is from sewage.
    In this study, one-step in situ microwave-assisted headspace solid-phase microextraction (MA-HS-SPME) followed by gas chromatography-mass spectrometry (GC-MS) analysis is presented as a fast and solvent-free technique
    to determine synthetic polycyclic musks in sewage sludge, sediment and oyster samples. The dewatered solid sample mixed with 20-mL deionized water was efficiently extracted by a polydimethylsiloxane-divinylbenzene (PDMS-DVB)
    fiber placed in the headspace when the extraction slurry was microwave irradiated at 80 W for 5 min. The limits of detection (LODs) ranged from 0.04 to 0.1 ng/g, and the limits of quantification (LOQs) ranged from 0.1 to 0.3 ng/g
    (fresh weight).
    A preliminary analysis of those samples revealed that HHCB and AHTN were the two most commonly detected synthetic polycyclic musks; using a standard addition method, their total concentrations were determined to rangefrom 0.3 to 10.9 ng/g (fresh weight) with relative standard deviation (RSD)ranging from 4% to 10%.
    The analytical procedure developed demonstrated that the MA-HS-SPME and GC-MS-SIM methods are reliable, sensitive and offer a convenient analytical technique for trace determination of polycyclic musks in various solid
    samples in environment.

    第一章 前言 1 1-1 研究緣起 1 1-2 研究目標 5 第二章 文獻回顧 6 2-1 新興污染物 6 2-1-1 新興污染物的來源及環境流佈 6 2-1-2 多環類麝香化合物簡介 10 2-1-3 多環類麝香化合物的毒性與物化性質 12 2-1-4 多環類麝香化合物的污染現況 17 2-1-5 相關研究文獻 19 2-2 微波輔助萃取法 22 2-2-1 微波簡介 22 2-2-2 加熱原理 24 2-2-3 微波裝置 26 2-2-4 微波的應用 27 2-3 固相微萃取法 30 2-4 氣相層析質譜儀 35 2-4-1 四極矩質譜儀 38 2-4-2 選擇離子偵測法 39 2-5 標準添加法 40 第三章 實驗步驟與樣品分析 43 3-1 實驗藥品與設備 43 3-1-1 實驗藥品 43 3-1-2 儀器設備 44 3-2 實驗步驟 46 3-2-1 標準品的配製 46 3-2-2 氣相層析質譜儀的參數設定 46 3-2-3 MA-HS-SPME裝置示意圖 48 3-2-4 微波輔助頂空固相微萃取步驟 49 3-3 樣品採集 50 3-2-1 底泥採集 50 3-2-2 牡蠣樣品收集 50 3-4 真實樣品檢測定量步驟 51 第四章 結果與討論 52 4-1 氣相層析質譜儀對多環類麝香化合物之分析 52 4-1-1 多環類麝香化合物標準品的測定 52 4-1-2 多環類麝香化合物標準品的儀器偵測極限與線性範圍 57 4-2 微波輔助萃取條件最佳化 58 4-2-1 微波瓦數對於萃取量的影響 58 4-2-2 萃取時間對於萃取量的影響 59 4-3 模擬樣品的最佳化 61 4-3-1 萃取溶劑體積對於萃取量的影響 61 4-3-2 NaCl添加量 62 4-3-3 pH值對於萃取量的影響 64 4-4 微波輔助頂空固相微萃取法的最佳化結果 66 4-3-3 微波輔助頂空固相微萃取法之最佳化條件 66 4-4-3 微波輔助頂空固相微萃取法之檢量線 67 4-5 微波輔助萃取法與傳統萃取方法的比較 69 4-6 環境樣品中多環類麝香的定量分析 71 4-6-1 底泥樣品中多環類麝香化合物的測定 71 4-6-2 牡蠣樣品中多環類麝香化合物的測定 77 第五章 結論與建議 79 5-1 結論 79 5-2 建議 80 第六章 參考文獻 81

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