本計畫擬研究含氮雜環六氫吡啶與唑類衍生物之測定與快速檢測器之研究，其目標如下： 第一年： 利用電沉積方法製備金與銀、金與鉑和金與鈀奈米二元合金。用掃描電子顯微鏡(SEM), 能量分散 (EDX), x-射線光電子光譜(XPS)等觀察這些奈米二元金屬電極表面微觀形態與金屬樹突微結構。以循環伏安法(CV)和高效率液相層析連結電化學檢測器(奈米二元合金)評估含氮雜環與其金屬衍生物反應機構與檢測器電催化效率。設計檢測器測定實際樣品(化妝品與藥品)中含氮雜環衍生物含量。 第二年： 研究硒化合物金和銀電極上自組薄膜當檢測器之工作電極。利用紅外反射吸收光譜(IRRAS)偵測 Se- Au 與 Se-Ag 鍵結變化 (相對穩定性)。Se-SAM 修飾電極用電化學交流阻抗光譜法 (EIS)和循環伏安法 (CV) 研究電極表面特性。並連線電化學與石英晶體微天平儀器 (EQCM)評估 Se-SAM 膜厚度。 除此，高效率液相層析連結電化學檢測器 (Se-SAMs)，研究合適電化學參數。同時串聯紫化光感測器測定氮雜環衍生物，並比較結果。第三年：奈米金屬(Ag, Pt)電沉積於單或多管壁之奈米碳管修飾玻璃碳電極上，製備複合體檢測器。使用感度高有預濃度效果的微分脈衝剝除伏安法 (DPSV)測定含金屬藥物。製作流動式電解槽-連接感測器(奈米金屬/奈米碳管/玻璃碳電極)與電化學儀器，此系統用於研究藥物的吸附動力學與含量測定。評估各種參數如電解質、pH 與流速，對感測器在流動式電解槽之影響。此系統可同時獲得藥物的電位、電流變化值，與電流對時間關係圖。將複合體感測器與紫化光感測器串聯於液相層析儀，測定化妝品與藥品中金屬含硫雜環衍生物之藥物含量。 The project is proceeding with the construction study of nitrogen - containing heterocyclic piperidine and azole derivatives in cosmetics and drugs. The objects are the following as: First year: Silver-gold (Ag-Au), gold-platinum (Au-Pt) and gold-palladium (Au-Pd) bimetallic nanoalloys are prepared by electrodeposition methods. The surface morphologies and crystal nanostructures of the dendrites are characterized a scanning electron microscope (SEM), energy dispersive X-ray spectroscopy (EDX), and x-ray photoelectron spectroscopy (XPS). The cyclic voltammetry (CV) and high-performance liquid chromatography (HPLC-ECD) with an electrochemical (bimetallic alloyed nanoparticles (NPs) detector are employed to evaluate the reaction mechanism of nitrogen heterocycles and metal derivatives and the electrocatalytical performance for sensor. The designed sensor is studied to test in a real drugs and cosmetics sample for the determination of nitrogen heterocycles. Second year: Design of selenium based self-assembled monolayers (SAMs) as chemical sensor used to this study is of substituted alkaneselenolate and aromatic selenolate, on gold and silver substrates, respectively. The relative stability of Se- Au and Se-Ag bonding is monitored using infrared reflection absorption spectroscopy (IRRAS).The composite of the Se - SAMs modified electrode is characterized by electrochemical impedance spectroscopy (EIS) and cyclic voltammatry (CV). The electrochemical behavior of nitrogen heterocycles using Se-SAMs electrode is studied by electrochemical quartz crystal microbalance (EQCM) and evaluated film thickness. In addition, nitrogen heterocycles is detected using high-performance liquid chromatography with an electrochemical (Se-SAMs) detector (HPLC-ECD). For direct current mode, with the current at a constant potential, and measurements with suitable experimental parameters using HPLC-ECD and HPLC with an ultraviolet detector is compared. Third year: Metal such as silver and platinum nanoclusters were electrochemically deposited on the single or multi-walled carbon nanotube modified glassy carbon electrode (Metal nano /CNTs/GCE), which fabricated a metal-CNTs composite sensor to detect metal- contaning heterocyclyes. In this study is to investigate the electrochemical behavior of metal heterocycles drugs on the Metal nano /CNTs/GCE, and to develop a sensitive stripping (preconcentration step) followed differential pulse voltammetric quantification. Design a flow – through Metal nano /CNTs/GCE sensor for measure and adsorption studies. The response of the Metal nano /CNTs/GCE to different parameters such as electrolyte, pH and flow rate in the flow cell was evaluated. Simultaneous measurements of potential-current or current-time transients allowed investigated of nitrogen heterocycles and metal derivatives electrochemical processes.
