第一部分研究為利用液高效能液相層析法結合感應耦合電漿質譜儀，對食物樣品中之Cr(VI)進行分析。為了減輕來自背景的40Ar12C+與40Ar12CH+等的多原子離子光譜干擾，使用動態反應槽 ( Dynamic reaction cell ) 搭配NH3做為反應氣體，將干擾物反應成中性來減少干擾。在液相層析法中使用陰離子交換樹脂( Anion-exchange chromatography ) PRP-X100作為管柱，以硝酸銨作為動相以分離Cr(III)與Cr(VI)，整體分析時間可於7分鐘內進行完成，Cr(VI)可得到0.067 ng mL-1之偵測極限，滯留時間、波峰高度與波鋒面積之再現性RSD皆優於3.2%。本研究利用鹼性溶液來進行萃取，在鹼性溶液中Cr(VI)比較穩定，可以避免鉻物種發生轉變，最後選用四甲基氫氧化銨 ( TMAH ) 為萃取試劑，並使用超音波震盪輔助萃取，最後將本方法應用於糖尿病保健食品、魚類與麵包中Cr(VI)的分析應用。

第二部分為利用液相層析法結合感應耦合電漿質譜儀對食品中的含硫化合物進行分析。由於感應耦合電漿質譜儀偵測硫會有很嚴重的光譜干擾，研究中選用O2做為動態反應槽的反應氣體，將32S與34S反應成32S16O與34S16O進行分析。在液相層析中使用陰離子交換層析法，將sulfite ( SO32- )、sulfate ( SO42- )及thiosulfate ( S2O32- )三種硫化合物分離，分析中為了使SO32-穩定，會在動相硝酸銨中添加甲醛使sulfite衍生化。整體分析時間5分鐘內分離SO32-、SO42-及S2O32-，可得到51 -62 ng mL-1之偵測極限。滯留時間、波峰高度與波鋒面積之再現性RSD皆優於3.7%。選用動相硝酸銨為萃取試劑，並使用超音波震盪輔助萃取，隨後用標準參考樣品NIST1573a Tomato Leaves進行方法的驗證，最後將此方法應用於金針花與巴西蘑菇樣品中含硫化合物的分析應用。

First part of research focused on HPLC-ICP-MS for the determination of Cr(VI) in food samples. The interfering 40Ar12C+ and 40Ar12CH+ ions were reduced by using NH3 as reaction cell gas. The separation was performed by using anion-exchange liquid chromatography on a PRP-X100 column with 50 mM Ammonium nitrate (NH4NO3) and 1%(v/v) MeOH at pH 9.8 as a mobile phase. The overall analysis time this can be applied to within 7 minutes. The detection limits for Cr(VI) was found to be 0.067 ng mL-1. We were explored various other factors such as reproducibility of retention time, peak height and peak area were better than 3.2% RSD. In our experiment we were used alkaline solution to the extraction process, Cr(VI) is relatively stable in the alkaline conditions. The selections of TMAH as the extraction reagent was used by ultrasound assisted extraction techniques followed by this determine Cr(VI) in diabetes healthly food, fish and bread samples.

Second part of research methodology focused on HPLC-ICP-MS for the determination of sulfur containing compounds in food samples. The determination of sulfur compound ( S32 and S34 ) in ICP-MS techniques which had serious spectral interference, in order to avoid this problem we used dynamic reaction cell by oxygen (O2) as a reaction gas to determine the analysis ( 32S16O and 34S16O ). The separation was performed using anion-exchange liquid chromatography on a PRP-X100 column with 60 mM Ammonium nitrate (NH4NO3) and 0.1% (v/v) formaldehyde at pH 7.0 as mobile phase. The overall analysis time this can be applied to within 5 min. The detection limits for SO3- , SO42- and S2O32- were found to be 51-65 ng mL-1. Reproducibility of retention time, peak height and peak area were better than 3.7% RSD. The mobile phase was used as extraction reagent by ultrasound assisted extraction techniques. The method was applied and then validated by standard reference sample NIST1573a Tomato Leaves. Finally, this method was applied to lily flower and mushroom samples.

論文審定書 i
謝誌 ii
摘要 iii
Abstract iv
目錄 vi
圖目錄 xiii
表目錄 x

第一章 液相層析結合感應耦合電漿質譜儀於食物樣品中Cr(VI)之分析應用
壹、 前言 1
貳、 實驗部分 4
一、 儀器裝置 4
二、 藥品與溶液的配製 5
參、 實驗過程 7
一、 液相層析分離條件探討 7
二、 DRC-ICP-MS系統最適化探討 8
三、 再現性 9
四、 校正曲線及偵測極限 9
五、 萃取條件最適化探討 10
六、 樣品配製 10
肆、 結果與討論 14
一、 液相層析條件之分離條件最適化 14
二、 DRC-ICP-MS系統最適化探討 21
三、 再現性 28
四、 校正曲線及偵測極限 28
五、 萃取條件最適化探討 28
六、 真實樣品的分析 41
伍、 結論 52
陸、 參考文獻 53

第二章 液相層析結合感應耦合電漿質譜儀於食物樣品中含硫化合物之分析應用
壹、 前言 57
貳、 實驗部分 60
一、 儀器裝置與設備 60
二、 試藥與溶液的配製 60
參、 實驗過程 62
一、 液相層析分離條件探討 62
二、 DRC-ICP-MS系統最適化探討 62
三、 再現性 63
四、 校正曲線及偵測極限 63
五、 萃取條件最適化 64
六、 樣品配製 64
肆、 結果與討論 68
一、 液相層析條件之分離條件最適化 68
二、 DRC-ICP-MS系統最適化探討 74
三、 再現性 84
四、 校正曲線及偵測極限 84
五、 萃取條件最適化 84
六、 真實樣品的分析 87
伍、 結論 100
陸、 參考文獻 101

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