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研究生: 周瑞琦
Chou, Ruei-Chi
論文名稱: 利用濾膜過濾、鉗合萃取技術和石墨爐式原子吸收光譜法進行尿液中錳元素的物種分類
Speciation of Manganese in Urine by Membrane Filtration,Chelating Extraction and Graphite Furnace Atomic Absorption Spectrometry
指導教授: 吳家誠
Wu, Jia-Cheng
學位類別: 碩士
Master
系所名稱: 化學系
Department of Chemistry
論文出版年: 2001
畢業學年度: 89
語文別: 中文
中文關鍵詞: 石墨爐式原子吸收光譜法尿液物種分類
英文關鍵詞: Manganese, GFAAS, urine, Speciation
論文種類: 學術論文
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  • 錳是人體所必須的微量元素,同時它也是已知的神經毒性物質。當人暴露於高濃度錳的環境中時,會造成身體的傷害及罹患疾病。錳中毒的病人會出現與帕金森氏症相似的病症,故錳被懷疑與此種疾病有關。
    由於錳被廣泛應用在鋼鐵工業上、電池中、殺蟲劑及油漆成份等等,在日常生活中有很多機會接觸到含錳的物質。適量的錳是人體所必須的,而過量的錳卻會造成人體的傷害。所以錳以必要的檢測技術去瞭解是相當重要的。
    鑑於文獻中有關有機態錳物種的分析報導甚少,早期的文獻大多檢測生物樣品的總錳含量。本實驗係將尿液分成七類物種分析:全量尿液中的錳物種、液相尿液中的錳物種、固相尿液中的錳物種、液相尿液中的鉗合性錳物種及非鉗合性錳物種、全量尿液中的鉗合性錳物種及非鉗合性錳物種七類物種。分類的技術主要是利用薄膜過濾,將尿液分成全量、液相及固相三類。另外,前兩類再利用Chelex-100樹脂的鉗合萃取特性,將可鉗合的二價錳離子留置在樹脂中,再利用酸萃出分析;其餘的非鉗合性錳物種,以微波消化的方式,將其轉變為可鉗合的二價錳離子,再利用上述步驟分析。因此共可分成七類錳物種。實驗結果顯示,人體尿液中存在的錳以液相尿液中的錳含量最高,佔尿液中總錳含量的 70 % 以上。而液相尿液中鉗合性錳物種於液相尿液中,分佈的比例規律性不高。但是可以發現將近五成液相尿液樣品中,鉗合性的錳物種佔90 % 以上。表示在液相尿液中二價錳離子的存在是居大多數的。在分析方法的精密度與準確度方面,以標準參考尿液 ( SRM-2670 ) 經過消化及Chelex-100管柱前濃縮後,再利用石墨爐式原子吸收光譜儀偵測,以確認精密度與準確度。

    Manganese is an essential trace element for mammals; however, exposed to high concentrations of manganese, human’s body could get certain diseases due to its neurotoxic excess. Some of these effects are irreversible. Extremely high concentration of manganese will induce Manganese intoxication and the symptoms are similar to those of Parkinson’s disease. Therefore, manganese is considered to be possibly related to Parkinson’s disease. Manganese is widely applied in the processes of manufacturing of iron alloys, dry batteries and is also found in many organo-manganese compounds. Not much information can be obtained on the distribution and speciation of manganese in human body. Therefore, it’s important to develop techniques to determine and speciate manganese in human’s body.
    In this study, Graphite Furnace Atomic Absorption Spectrometry ( GFAAS ) is used to determine manganese in the urine. We use membrane filtration and chelating extraction techniques to speciate manganese in urine samples. We can define seven manganese species with analytical procedures-total manganese in urine, solid form of manganese in urine, soluble form of manganese in urine, chelating-extractable manganese in liquid urine, non-chelating-extractable manganese in liquid urine, chelating-extractable manganese in total urine and non-chelating-extractable manganese in total urine. Our research showed that more than 70% of the total manganese in urine was in soluble form and the rest was in solid form. The amount of manganese in soluble form of urine extractable with chelex-100 resin is irregular. The irregularity may relate to life style and diet habit of each individual. Spike recovery tests of EDTA-Mn in standard urine confirmed that stable organo-manganese does not react with chelex-100. The results from digested and column-preconcentrated standard reference urine confirmed the accuracy and precision of the analytical scheme.

    第一章 緒論 一、研究動機 ......................1 二、自然界存在的錳.................. .2 三、錳元素對人體的影響................ .3 四、帕金森氏病和帕金森氏症 ............. .4 五、錳的主要用途................... .5 六、錳的攝入來源................... .6 七、人體中錳元素的分佈................ .9 八、尿液樣品的選擇 .................. 9 九、無塵技術的必要性..................11 十、偵測生物樣品中的錳元素 .............. 12 十一、錳的一些有機鍵結物質...............15 第二章 實驗儀器、器材和試劑 一、儀器設備......................19 二、器材........................20 三、試劑........................22 第三章 實驗內容 一、試藥的配製與與純化.................25 二、器材清洗方式....................30 三、尿液錳元素分析...................30 (一) 尿液的採集.................. 30 (二) 尿液的保存................. .31 (三) 微波消化.................. .33 (四) 管柱前濃縮.................. 38 (I) Chelex-100管柱的製備............ .38 (II) Chelex-100管柱前濃縮程序...........38 (III) Chelex-100 樹脂管柱最適條件尋找...... .41 (五) 石墨爐式原子吸收光譜儀條件最佳化....... 46 (六) 儀器的偵測極限 ................48 四、尿液中錳物種的分類.................48 (一) 尿液中的總錳含量( TUMn )的測定........ 49 (二)液相尿液的錳含量( LUMn ) 的測定........ 49 (三)固相尿液的錳物種( SUMn ) 的測定........ 49 (四)全量尿液中的鉗合性錳物種( TUCMn ) 的測定.....................51 (五)全量尿液中的非鉗合性錳物種( TUNMn ) 的測定..................... 51 (六)液體尿液中的鉗合性錳物種( LUCMn ) 的測定..................... 51 (七)液體尿液中的非鉗合性錳物種( LUNMn ) 的測定.....................51 五、 鉗合性錳物種存在的確認.............. 52 六、 方法偵測極限及其確認.. .............54 七、 標準參考尿液的分析................ 55 八、 方法精密度與準確度................ 56 九、 真實尿液樣品的測定................ 57 第四章 結論 一、微波消化條件的探討.................61 二、Chelex-100樹脂管柱濃縮條件探討........ .. 63 三、檢量線結果的探討..................68 四、原子吸收光譜儀的昇溫條件探討........... 68 五、實驗各階段的空白..................79 六、物種分類流程的確認.................82 七、方法偵測極限及其確認 ............... 84 八、標準參考尿液的分析....................84 九、方法的精密度與準確度 ............... 86 十、真實尿液結果的探討 ................ 86 第五章 結果與討論 ......................99 第六章 參考資料...................... 102

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