本文選題：非水毛細(xì)管電泳 + 電化學(xué)發(fā)光��； 參考：《鄭州大學(xué)》2014年碩士論文

【摘要】：非水毛細(xì)管電泳(NACE)是指在有機(jī)溶劑中進(jìn)行的電泳操作，與水相毛細(xì)管電泳(CE)相比，電泳電流低，樣品處理簡單，與電化學(xué)檢測器兼容性更好。NACE能夠用來分離在水相中不能分離的中性物質(zhì)、難溶于水的物質(zhì)以及在水中不穩(wěn)定的物質(zhì)。電化學(xué)發(fā)光(ECL)是指通過施加電壓，電極表面的物質(zhì)發(fā)生反應(yīng)，產(chǎn)生電子轉(zhuǎn)移，產(chǎn)生發(fā)光的現(xiàn)象。其中，三聯(lián)吡啶釕發(fā)光試劑不論在水相還是有機(jī)相中都具有溶解性好、性質(zhì)穩(wěn)定、發(fā)光試劑可循環(huán)利用等優(yōu)點(diǎn)，在電化學(xué)發(fā)光（ECL）中的應(yīng)用最廣泛。本文將NACE與ECL檢測相聯(lián)用，檢測含三級(jí)胺結(jié)構(gòu)的藥物： 1、合成高氯酸根型Ru(bpy)3(ClO4)2發(fā)光試劑替代傳統(tǒng)的氯離子型Ru(bpy)3Cl2發(fā)光試劑，并其應(yīng)用于NACE-ECL技術(shù)中，克服氯離子對(duì)發(fā)光信號(hào)的干擾，得到非常強(qiáng)的ECL信號(hào)，我們用三丙胺(TPrA)來表征乙腈相中Ru(bpy)3(ClO4)2的靜態(tài)ECL信號(hào)。當(dāng)加入1mM TPrA后，ECL信號(hào)明顯增強(qiáng)，大約為不加時(shí)信號(hào)的400倍。實(shí)驗(yàn)中使用有機(jī)溶劑替代水溶液，Pt工作電極表面不容易產(chǎn)生氧化膜，無需活化處理，ECL信號(hào)的重現(xiàn)性非常好。將此發(fā)光試劑應(yīng)用于毛細(xì)管電泳柱端檢測中，對(duì)于提高分析物的檢測效果具有潛在的應(yīng)用價(jià)值。 2、利用NACE-ECL聯(lián)用檢測技術(shù)分析檢測TPrA。研究發(fā)現(xiàn)：在5×10-9~1×10-5mol/L范圍內(nèi)ECL信號(hào)與TPrA濃度呈良好的線性關(guān)系，相關(guān)系數(shù)r=0.9992，最低檢測限為5×10-9mol/L。由于可以施加了分離電壓和使用短的毛細(xì)管柱（33cm），此方法可實(shí)現(xiàn)對(duì)TPrA快速分析檢測。 3、將NACE-ECL聯(lián)用技術(shù)應(yīng)用于琥珀酸多西拉敏、馬來酸非尼拉敏及其混合物的分析檢測，同時(shí)考察分離溶劑對(duì)這兩種藥物的分離效果。結(jié)果發(fā)現(xiàn)，當(dāng)混合溶劑DMF:ACN體積為40:60時(shí)，分離效果最好。 本文使用EC法在玻碳電極(GC)表面沉積不同的形態(tài)的Cu2O晶體，，有超級(jí)八面體、八面體和微球體結(jié)構(gòu)。將微球結(jié)構(gòu)的Cu2O-GC應(yīng)用于葡萄糖傳感器中，表現(xiàn)出良好的電催化性能。
[Abstract]:Non-aqueous capillary electrophoresis (NACE) refers to electrophoretic operation in organic solvents. Compared with aqueous capillary electrophoresis (CEE), the electrophoretic current is lower and sample handling is simple. NACE can be used to separate neutral, insoluble and unstable substances in water. Electrochemiluminescence (ECL) refers to the phenomenon of electron transfer and luminescence by applying voltage to the material on the electrode surface. Among them, tripyridine ruthenium luminescence reagents have many advantages, such as good solubility, stable properties and recycling of luminescence reagents, both in aqueous and organic phases, so they are widely used in electrochemical luminescence (ECL). In this paper, NACE was combined with ECL to detect drugs with tertiary amine structure. 1. The synthesis of perchlorate type RubpyN 3CIO 4 O 4 O 2 luminescent reagent instead of the traditional chlorine ion type RubpyN 3Cl 2 luminescent reagent was applied in NACE-ECL technology. A very strong ECL signal was obtained by overcoming the interference of chloride ions to the luminescent signal. The static ECL signal of RunbpyN _ 3CIO _ 4N _ 2 in acetonitrile phase was characterized by tripropylamine (TPRA). When 1 mm TPrA was added, the ECL signal was obviously enhanced, which was about 400 times of that of the undelayed signal. In the experiment, it is not easy to produce oxide film on the surface of Pt electrode by using organic solvent instead of aqueous solution, and the reproducibility of ECL signal without activation is very good. The application of the luminescent reagent in capillary electrophoresis column end detection has potential application value for improving the detection effect of the analyte. 2. The detection of TPrA by NACE-ECL is carried out by using NACE-ECL. It is found that there is a good linear relationship between ECL signal and TPRA concentration in the range of 5 脳 10 ~ (-9) mol / L ~ (-1) 脳 10 ~ (-5) mol / L, the correlation coefficient is 0.9992, and the detection limit is 5 脳 10 ~ (-9) mol / L. Because the separation voltage can be applied and a short capillary column can be used to detect TPrA, this method can be used for the rapid analysis and detection of TPrA. 3. The NACE-ECL technique was applied to the analysis and detection of doxillamine succinate, fenilamine maleate and its mixture. At the same time, the separation effect of separation solvent on these two drugs was investigated. The results show that the separation efficiency is the best when the volume of DMF: ACN is 40:60. In this paper, different forms of Cu2O crystals have been deposited on the surface of glassy carbon electrode (GC) by EC method, with super octahedron, octahedron and microsphere structure. Cu2O-GC with microsphere structure was applied to glucose sensor and showed good electrocatalytic performance.
【學(xué)位授予單位】：鄭州大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2014
【分類號(hào)】：R917

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