利用混合吸附劑故項萃取法結合液相層析串聯質譜技術檢測水樣中人工代糖的濃度

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李岱庭(Dai-Ting) 查詢紙本館藏

畢業系所

化學學系

論文名稱

利用混合吸附劑故項萃取法結合液相層析串聯質譜技術檢測水樣中人工代糖的濃度

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摘要(中)

本研究使用自行填充的HLB (Hydrophilic-Lipophilic Balance) 及C18混合吸附劑進行固相萃取 (Solid Phase Extraction, SPE) ，並使用液相層析串聯質譜儀 (Liquid Chromatography - Tandem Mass Spectrometry, LC-MS/MS)進行水樣中三氯蔗糖及阿斯巴甜的偵測，偵測極限分別為14 ng/L與10 ng/L，定量極限分別為120 ng/L與78 ng/L。本研究同時使用"面中心中央合成設計 (Face-Centered Center Composite Design, FCCCD) 進行多因子實驗條件最佳化法，可減少實驗次數以及可觀察因子間的交互作用關係。最佳化條件如下:固相萃取匣吸附劑重量為180 mg，比例為HLB:C18 = 3:1，進樣流速為2.5 mL/min，沖提溶劑為甲醇，體積為15 mL。使用Mandel’s Fitting Test及Lack of Fit測試檢量線及實驗設計模型的適用性，並進行再現性測試相對標準偏差均小於7%。
　　本研究檢測自來水，瓶裝水，地下水與河流水水樣，這是國內首次有關人工代糖在飲用水與環境水樣中的檢測結果，其中三氯蔗糖濃度為3.6 μg/L至31 μg/L，阿斯巴甜皆無檢出，除一個河流水水樣濃度為2.7 μg/L；本研究所開發混和型固相萃取搭配液相層析串聯質譜儀具有良好的靈敏度及穩定性，可應用於不同水樣來源的濃度檢測。

摘要(英)

In this study hybrid-SPE was applied to extract Artificial Sweeteners (ASs) from various water samples. Combination of HLB (Hydrophilic-Lipophilic Balance) and ENVI-C18 was applied as the adsorbent for hybride-SPE, and the factors affecting the extraction efficiency of the analytes were optimized by a Face-Centered Central Composite Design (FCCCD). Optimized extraction conditions were as follows: adsorbent ratio HLB: ENVI-C18 = 3:1, adsorbent amount: 180 mg, sampling flow rate: 2.5 mL/min, and elution solvent: 15 mL methanol. The SPE extractant was then analyzed by HPLC – MS / MS. Limits of quantitation (LOQ) were 120 ng/L and 78 ng/L for sucralose and aspartame, respectively. In this study we analyzed tap water, bottled water, groundwater and river water samples, this is the first report of ASs detection in Taiwan. Sucralose concentrations were ranged from 3.6 to 31 μg/L, and aspartame was only detected in one river water sample, its concentration was 2.7 μg/L. In this study, efficient and reliable hybrid-SPE coupled with HPLC-MS/MS procedure was developed, which is sensitivity, stability, and can be applied in analysis of ASs in various of water samples.

關鍵字(中)

★ 人工代糖
★ 液相層析儀
★ 串聯質譜

關鍵字(英)

論文目次

目錄
摘要 I
Abstrat II
謝誌 III
目錄 V
圖目錄 IX
表目錄 XIII
第一章　前言 1
1-1　研究緣起 1
1-2　研究目標 3
第二章　文獻回顧 5
2-1　人工代糖 5
2-1-1 人工代糖的性質 7
2-1-2 文獻回顧 10
2-2高效液相層析質譜儀 14
2-2-1 電噴灑游離法 17
2-2-2 離子阱質量分析器原理 22
2-3 固相萃取法 24
2-4 實驗的統計設計 27
2-4-1 統計實驗設計簡史 27
2-4-2 變異數分析 29
2-4-3 因子設計 31
2-5品質保證與品質管制 33
2-5-1 分析數據的品質 33
2-5-2 品質保證系統 34
2-5-3　檢量線確認 36
2-5-4　缺適性測試 38
2-5-5 基質效應 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 45
3-2　實驗步驟 46
3-2-1　標準品的配製 46
3-2-2　人工代糖的檢測 47
3-2-3　水樣之萃取步驟 50
3-3　水樣採集 52
第四章　結果與討論 53
4-1 液相層析質譜儀對人工代糖之分析 53
4-1-1 毛細管電壓(Capilliary Voltage)對待測物感度之影響 53
4-1-2 串聯質譜定量分析 56
4-1-3 儀器的偵測極限 60
4-2 固相萃取最佳化條件探討 62
4-2-1 固相萃取管柱的選擇 62
4-2-2 吸附劑比例的選擇 65
4-2-3 固相萃取實驗設計最佳化 66
4-3 檢量線確認 73
4-4 真實樣品檢測 75
4-4-1 真實樣品檢測結果 75
4-4-2 方法確效 82
4-4-3 基質效應檢視 83
第五章　結論 85
第六章　參考文獻 87

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指導教授

丁望賢(Wang-Hsien Ding)

審核日期

2013-7-5

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