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研究生: 黃芷婷
論文名稱: 食品中多重重金屬的微量分析
Trace Analysis of Multi Elements in Foods by ICP-MS
指導教授: 凌永健
口試委員: 吳家誠
劉銘龍
凌永健
學位類別: 碩士
Master
系所名稱: 理學院 - 化學系
Department of Chemistry
論文出版年: 2013
畢業學年度: 101
語文別: 中文
論文頁數: 154
中文關鍵詞: ICP-MS微波消化食品攝入量不確定度現況調查
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  • 食物是人類攝取必需微量元素以及有毒元素的主要來源,本研究利用微波消化系統結合感應耦合電漿質譜儀(ICP-MS)應用於稻米中重金屬的總量分析研究,針對多重元素(As, Hg, Pb, Cd, Cu, Cr, Ni, Zn, Se, Al, In, Ga, Mo, W)進行微波消化以及ICP-MS的參數最適化評估。經實驗後選用6 mL conc.HNO3以及3 mL 30%(v/v)H2O2之混合溶液作為最佳消化溶液,於110 ℃的消化溫度下進行消化10分鐘,再根據不同之金屬元素選擇不同之上機模式進行偵測,經NIST標準品進行方法確效得回收率介於80~120 %間,並使用Top-down approach評估此方法之量測不確定度,介於0.08-5.08 mg/kg的範圍內。
    本研究收集來自全台75件白米樣品、25種魚類樣品以及42件豬肉樣品,進行現況樣品調查以及我國成年人及國小學童之週/日/月攝入量之評估。由數據結果顯示,75件白米樣品皆符合我國食品藥物管理署(食藥署)針對重金屬鉛、鎘、汞的規範;25種魚類樣品中濃度較高的砷及汞則需進一步建立物種分析方法以確認其中毒性較高之無機砷以及甲基汞的濃度;42件豬肉樣品則是都符合了食藥署針對可食用性家畜類內臟重金屬之規範。攝入量評估方面,我國國小學童各元素之週/日/月攝取量皆符合聯合國糧農組織以及世界衛生組織所制定之規範;成年人則是砷和汞有超標的情形。


    Food is the main way of intake of trace elements by human, and rice is the most important food that Taiwanese eat every day. This research aimed to construct a simple, fast and reliable method to analyze multi trace elements in rice by using inductively coupled plasma mass spectrometer, ICP-MS. Prior to instrumentalanalysis, microwave digestion system was successfully applied to decompositionof samples by using 6 ml of concentrated nitric acid and 3 ml of 30 % hydrogen peroxide under 10 minutes and 110 ℃digestion. To validate the proposed method, three Standard Reference Materials from the National Institute of Standard and Technology,were analyzed, and the recovery of each element was in the range of 80-120 %. The measurement uncertainty was alsoevaluated by top-down approach, and the results are in the range of 0.08-5.08 mg/kg.
    Afterwards, 75 rice samples from different regions in Taiwan, 25 different species of fish samples and 42 pork samples were collected as field research samples. Finally, the provisional tolerable weekly/daily/monthly intake of adults and elementary childrenwere estimated. All of the 75 rice samples and 42 pork samples are under the regulation for heavy metals set by Food and Drug Administration. Further speciation method is needed for fish samples to check the concentration of inorganic arsenic and methyl mercury. Average weekly/daily/monthly intake of each element of elementary children is under the regulation set by World Health Organization, but the weekly intake of arsenic and mercury of adults are above the regulation.

    摘要 I Abstract II 目錄 III 表目錄 VII 圖目錄 XI 第一章緒論 1 1.1 前言 1 1.2 研究動機及目的 2 第二章文獻整理 3 2.1 重金屬 3 2.1.1 鋁(Aluminum) 3 2.1.2 鋅(Zinc) 4 2.1.3 鉻(Chromium) 4 2.1.4 鎳(Nickel) 5 2.1.5 銅(Copper) 5 2.1.6 砷(Arsenic) 5 2.1.7硒(Selenium) 6 2.1.8 鎘(Cadmium) 6 2.1.9 鉛(Lead) 7 2.1.10 汞(Mercury) 7 2.2 重金屬管制規範 8 第三章多重元素總量分析方法建立 13 3.1 實驗目的 13 3.2 實驗原理 13 3.2.1 微波消化(Microwave Digestion) 13 3.2.2 感應耦合電漿質譜術(Inductively Coupled Plasma Mass Spectrometry) 14 3.2.3 量測不確定度(Measurement Uncertainty) 19 3.3 實驗設備及藥品 23 3.3.1 設備 23 3.3.2藥品 23 3.3.3 溶液配製 23 3.4 實驗方法 25 3.4.1優化微波消化條件 25 3.4.2 ICP-MS分析 26 3.4.3品保品管 27 3.4.4評估量測不確定度 29 3.5 結果與討論 30 3.5.1 微波消化最佳化條件 30 3.5.2 方法確效 30 3.5.3 量測不確定度 32 3.6 結論 33 第四章現況調查 70 4.1 實驗目的 70 4.2 樣品採集 70 4.3 實驗方法 70 4.4結果與討論 71 4.5 樣品之週/日/月攝取量評估 75 4.6 稻穀各部位濃度分析 82 4.7結論 83 第五章參考文獻 151

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