第一部分研究採用離子對逆相層析法(Ion pair reverse phase chromatography)結合感應耦合電漿質譜儀針對菸草及菸灰樣品中的鉈（Tl）進行物種分析。實驗中先以動態反應槽結合感應耦合電漿質譜儀得知菸草及菸灰中鉻、鎳、砷、鎘、鉈及鉛的濃度。層析系統為使用C8管柱，並以Tetra-n-butylammonium phosphate (TBAP)作為離子對試劑；Diethylenetriamine -pentaacetic acid (DTPA)做為螯合試劑。經條件最適化探討後，動相最適化條件組成為7 mM TBAP、6 mM DTPA、2%(v/v)甲醇，pH值5，流速1.0 mL min-1，可於2分鐘內快速分離Tl(I)及Tl(III)。此條件下獲得Tl(I)及Tl(III)的偵測極限皆低至3 ng L-1，層析峰面積再現性RSD值為1% ( n = 5 )。菸草樣品則為選擇台灣、日本、美國三種產地之菸草，使用100 mM醋酸銨、5 mM DTPA為萃取試劑，以超音波振盪20分鐘，為一簡單、快速及價格不高的萃取方法，其萃取效率達98%以上。同時也針對台灣產地香菸之菸灰進行萃取，使用100 mM醋酸銨、5 mM DTPA菸草萃取試劑加上2%(v/v) HF，以超音波振盪20分鐘，其萃取效率介於94-105%。結果得知菸草樣品中皆為毒性較高的Tl(I)；菸灰樣品中同時存在Tl(I)及Tl(III)，菸草樣品添加回收率介於90-98%範圍之間，證明本研究方法的準確性及可行性。
第二部分研究利用泥漿進樣結合流動注入化學蒸氣生成技術結合感應耦合電漿質譜儀分析眼影中砷、鎘、銻、汞及鉛之含量。為得到最佳分析物訊號之靈敏度，實驗中依序對增益試劑thiourea濃度、Co濃度、HCl濃度、NaBH4濃度、反應試劑流速、混合線圈體積做最適化探討。實驗中比較水溶液校正法（External calibration﹚及標準添加法（Standard addition﹚之斜率，結果顯示基質會影響氫化物生成效率，故最後選擇標準添加法進行分析物之定量，並搭配同位素稀釋法驗證此方法。本研究所得砷、鎘、銻、汞及鉛之方法偵測極限分別為0.01、0.09、0.01、0.03、0.6 ng mL-1。由於眼影沒有標準參考樣品，因此採用乳霜標準參考樣品GBW 09305來驗證本研究方法之準確性。最後將以本研究方法分析三種不同顏色之市售眼影樣品，且同時比較使用同位素稀釋法、微波消化方法及ETV-ICP-MS所定量之結果來驗證方法準確性及可行性。

First part of research focused on an inductively coupled plasma mass spectrometry (ICP-MS) was used an ion pair reverse phase liquid chromatographic detector for the speciation analysis of thallium in tobacco samples. At first, the concentration of Cr, Ni, As, Cd, Tl, Pb was found by DRC-ICP-MS. An C8-HPLC column was used as the stationary phase; in addition to that, Tetra-n-butyl ammonium phosphate (TBAP) was used as an ion pair reagent followed by Diethylenetriamine-pentaacetic acid (DTPA) was used as a chelating reagent. The optimization conditions, were applied to 7 mmol L-1 TBAP, 6 mmol L-1 DTPA in 2% v/v methamol solution (pH=5) was used as a mobile phase, the separation was completed in less than 2 min and the detection limit was found to be 3 ng L-1 for both Tl(I) and Tl(III) compounds based on peak height. The relative standard deviation (RSD) of the peak areas for five injections (n=5) of a mixture containing Tl (1μg L-1) which showed better performance. Three kinds Tobacco samples were collected in various countries (Taiwan, Japan, USA) which was analyzed quantitatively for thallium species determination an optimized conditions as follows: tobacco with a 5 mmol L-1 of DTPA in 100 mmol L-1 ammonium acetate solution with ultrasonic bath in 20 min durations. This method was very simple, fast, cost effective and the extraction efficiency was better than 98%. In addition to improve the extraction efficiency furthermore we have enhanced with 5 mmol L-1 DTPA in 2% v/v hydrofluoric acid and 100 mmol L-1 ammonium acetate solution by ultrasonic bath in 20 min durations. The results which are shows that tobacco samples existed highly toxic Tl(I) species, and tobacco ash sample existed Tl (I)/(III) species. The spike recovery was achieved in 90-98% in order to prove the accuracy and feasibility of this method.
Second part of research methodology focused on, a slurry sampling with ICP-MS techniques to determine various elements such as As, Cd, Sb, Hg and Pb in eyeshadow commercial cosmetics sample using flow injection (FI) with vapor generation (VG) sample system. In the experiment, the concentration of thiourea, Co, HCl, NaBH4, reagent flow rate and mixing coil volume were optimized. The current study focused on, slope of external calibration and standard addition would be compared. The matrix of analyte could affect the hydride generation efficiency, so that the standard addition was chosen and detection limit was obtained from the curve in the range of 0.01-0.6 ng mL-1 for As, Cd, Sb, Hg and Pb. Since the eyeshadow didn’t have a standard reference material, the cream standard reference material GBW 09305 was used to verify the accuracy. Finally, three kinds of commercially available eyeshadow samples were analyzed by CVG-ICP-MS. At the same time, in order to prove the accuracy and feasibility of this method was verified by the isotope dilution/microwave digestion method with ETV-ICP-MS techniques.

論文審定書 i
謝誌 ii
摘要 iii
Abstract v
目錄 vii
圖目錄 x
表目錄 xii
第一章 液相層析結合感應耦合電漿質譜儀於菸草中微量毒性元素分析及鉈物種分析之應用
壹、 前言 1
一、 研究背景 1
二、 鉈元素之個論 1
三、 動態反應槽 3
貳、 實驗部分 5
一、 儀器裝置 5
二、 試劑藥品與溶液配製 7
參、 實驗過程 10
一、 液相層析分離條件探討 10
二、 再現性 11
三、 校正曲線、偵測極限的估計 11
四、 真實樣品分析 11
肆、 結果與討論 15
一、 ICP-MS於菸草及菸灰樣品鉻、鎳、砷、鎘、鉈及鉛定量分析 15
二、 液相層析條件最適化探討 18
三、 鉈物種的分析 24
四、 萃取條件 29
五、 HPLC-ICP-MS於真實樣品的分析 32
伍、 結論 42
陸、 參考文獻 43
第二章 流動式注入化學蒸氣技術結合感應耦合電漿質譜儀於眼影中微量元素分析之應用
壹、 前言 47
一、 研究背景 47
二、 金屬的毒性及對人體的危害 49
三、 流動注入法原理 50
四、 化學蒸氣生成法 51
五、 同位素稀釋法 54
貳、 實驗部分 56
一、 儀器裝置 56
二、 試劑藥品及溶液配製 58
參、 實驗過程 62
一、 化學蒸氣生成系統各參數之探討 62
二、 ICP-MS系統操作條件之探討 64
三、 樣品稀釋倍數之探討 64
四、 分析訊號之再現性 65
五、 光譜干擾探討 65
六、 校正曲線及偵測極限估計 67
七、 樣品前處理與分析 67
肆、 結果與討論 70
一、 化學蒸氣生成系統各參數之探討 70
二、 ICP-MS系統操作條件之探討 80
三、 樣品稀釋倍數之探討 80
四、 分析訊號之再現性 80
五、 光譜干擾探討 84
六、 校正曲線及偵測極限估計 84
七、 樣品前處理與分析 87
伍、 結論 95
陸、 參考文獻 96

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第二部分
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