自從微量元素的毒物學行為與生物化學的作用與其本身的化學形式有非常大的相關性被廣泛證實以來，時至今日，砷與汞物種的濃度分布情形在風險評估上已成為不可或缺的資訊。現今的文獻中，對於微量元素分析而言，光觸媒輔助還原蒸氣生成技術已被認為是一種靈敏且有效地分析技術。此外，近來一套靈敏、穩固並具有發展潛力的披覆式微流體晶片型奈米二氧化鈦光觸媒輔助蒸氣生成裝置 (nano-TiO2 μFPCAVD) 被成功開發並串連至連線分析系統中，且成功地應用於環境水體中微量無機硒物種的分析。為了擴展μFPCAVDs的性能，本研究利用μFPCAVDs串連建立三套連線分析系統分別針對環境水體與生物樣品中的微量汞與砷進行分析。
首先，本研究建立了一套microdialysis (MD)–nano-TiO2 μFPCAVD–inductively coupled plasma-mass spectrometry (ICP-MS) 連線分析系統，並應用於在硫柳汞 (TMHg) 暴露後，活體大鼠腦部組織細胞間液 (ECF) 中汞濃度的線上動態變化監測的分析研究上。在最適化操作參數條件下，本連線分析系統對於生理食鹽水中的甲基汞 (MMHg) 與TMHg的偵測極限 (limits of detection，LODs) 分別為2.7及1.7 ng L-1，並藉由與ICP-MS直測進行比較以評估系統的分析準確度。再經由實際應用於經MMHg與TMHg暴露後的活體動物腦部組織ECF中汞濃度的線上動態變化監測分析的方式進行MD–nano-TiO2 μFPCAVD–ICP-MS連線分析系統應用的可行性評估。由本研究的實驗結果可知，MD–nano-TiO2 μFPCAVD–ICP-MS可以有效地應用於活體動物腦部組織ECF中汞濃度的線上動態變化監測分析且其分析結果具有相當高的可信度。經由實驗數據發現暴露TMHg後所形成的含汞物質亦可以如MMHg般經由目前未知的途徑穿過血腦障壁進入腦部組織中。
其次，本研究亦建立了一套HPLC–nano-TiO2 μFPCAVD–ICP-MS連線分析系統，藉以針對環境水體中微量汞物種進行分析。藉由降低層析分離過程中的動相溶液流速與錯合試劑組成成分的濃度，在微量汞物種分析過程中，不僅能夠保持足夠好的汞物種分離效率更有效地控制了藥劑空白的汙染問題。在最適化操作參數條件下，本連線分析系統對於汞離子 (Hg(II)) 與MMHg的偵測極限 (LODs) 分別為0.52及0.58 ng L-1，並以標準參考樣品 (Seronorm™ trace elements urine L-2) 的分析評估系統的分析準確度。
最後，本研究亦發展了一套以披覆式微流體晶片型奈米複合材料光觸媒輔助蒸氣生成裝置 (nanocomposite μFPCAVD) 搭配高效能液相層析 (HPLC) 與感應耦合電漿質譜儀 (ICP-MS) 所建立的連線分析系統進行有選擇性且靈敏的分析方法針對微量無機砷物種進行分析。藉由奈米金的沉積針對nano-TiO2表面進行改質，使此奈米複合材料的光觸媒輔助還原效率可以有效提升。在最適化操作參數條件下，本連線分析系統對於無機三價砷 (As(III)) 與無機五價砷 (As(V)) 的偵測極限 (LODs) 分別為0.23及0.34 g·L−1，並以標準參考樣品 (NIST SRM 1643e) 的分析評估系統的分析準確度。
本研究所開發的連線分析系統亦實際應用於環境樣品或生物樣品的分析藉以進行真實樣品的可應用性評估。經實驗結果可知，本研究所開發的三套連線分析系統可以提供毒性及環境相關研究領域一系列具有發展潛力的分析方法。

Since it has been widely recognized that the toxicological behaviors and the biochemical functions of trace elements are highly dependent on chemical forms, the species information on arsenic (As) and mercury (Hg) is considered indispensable for the risk assessment. Over past decades, the utilities of photocatalyst-assisted reduction vapor generation techniques for the analysis of trace elements have been demonstrated. Afterward, the emergence of nano-TiO2 coated microfluidic-based photocatalyst-assisted vaporization device (nano-TiO2 μFPCAVD) hyphenated system provides not only a sensitive but also a robust analytical system for trace analysis of inorganic selenium species in natural water. To expand the capability, in this study, various analytical systems hyphenated with μFPCAVDs were developed for the determination of Hg and As at trace levels in natural water and biological samples.
For the first of the analytical systems, a microdialysis (MD)–nano-TiO2 μFPCAVD–inductively coupled plasma-mass spectrometry (ICP-MS) hyphenated analytical system was proposed for the in vivo quantification of the transition of Hg concentration level in the extracellular fluid (ECF) of rat brains after the administration of thimerosal (TMHg). Under optimal operation conditions, the limits of detection (LODs) for methylmercury (MMHg) and TMHg were 2.7 and 1.7 ng·L−1, respectively. The accuracy of the analytical results was validated using method comparison with ICP-MS detection. The applicability of the proposed analytical system was evidenced by the observations of the variation in the brain ECF Hg concentration in living animals after the administration of MMHg and TMHg. Based on the obtained results, the proposed analytical system exhibited satisfactory reliability and validity to monitor the transition of the ECF Hg concentration level. The results also indicated that the administration of TMHg can cause Hg-containing substances to penetrate through the blood–brain barrier as MMHg via an unclear mechanism.
Additionally, a high-performance liquid chromatography (HPLC)–nano-TiO2 μFPCAVD–ICP-MS hyphenated analytical system was developed for the Hg speciation analysis in natural water. With reduction of operation flow rate and complexing agent concentration in the mobile phase solution for chromatographic separation, either the separation efficiency and the reagent blank are well controlled for the determination of Hg species at trace level. Under optimal operation conditions, the LODs for mercuric ion (Hg(II)) and MMHg were 0.52 and 0.58 ng·L−1, respectively. The accuracy was validated using certified reference material (Seronorm™ trace elements urine L-2).
Ultimately, to achieve selective and sensitive determination of trace inorganic As species, i.e., As(III) and As(V), a nanocomposite μFPCAVD coupled with HPLC separation and ICP-MS detection was employed. Gold nanoparticles were deposited on nano-TiO2 to strengthen the conversion efficiency of the nanocomposite photocatalytic reduction. Under optimal operation conditions, the LODs for As(III) and As(V) were 0.23 and 0.34 μg·L−1, respectively. The accuracy was validated using certified reference material (NIST SRM 1643e).
The applicability was also established via the analysis of natural water samples or biosamples with all three proposed hyphenated analytical systems. Based on the obtained results, the proposed analytical systems can provide potential alternative methods for toxicological and environmental research.

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