本文選題：納米復(fù)合材料 + 修飾電極��； 參考：《上海大學(xué)》2016年博士論文

【摘要】：藥物分析是分析化學(xué)中的一個重要分支,隨著藥學(xué)的發(fā)展逐漸成為一門獨(dú)立的學(xué)科�，F(xiàn)代藥物分析無論是分析領(lǐng)域,還是分析技術(shù)都己經(jīng)大大拓展。電化學(xué)分析作為分析技術(shù)的一種,在藥物分析領(lǐng)域中有著日益廣泛的應(yīng)用。而各種微電極、修飾電極、電化學(xué)傳感器的問世,由于其具有靈敏度高、響應(yīng)快、選擇性好、操作簡單等優(yōu)點,為電化學(xué)分析在藥物分析中的應(yīng)用注入了新的活力。隨著工作者對電化學(xué)分析的研究日益深入,電化學(xué)分析在科研、生產(chǎn)中的應(yīng)用越來越廣泛,并且在新藥研發(fā)以及藥品生產(chǎn)等方面扮演著重要的角色。本論文主要研究了新型碳基納米材料復(fù)合修飾電極的制備,探索了不同藥物在修飾電極上的電化學(xué)行為和電極反應(yīng)機(jī)理,從而建立了一系列靈敏、簡單、準(zhǔn)確的藥物定量分析方法。主要內(nèi)容歸納如下:1、通過電化學(xué)方法將金屬氧化物四氧化三鈷(Co_3O_4)/石墨烯(GR)納米材料電沉積在玻碳電極表面上,制備了一種新型的納米復(fù)合電極(Co_3O_4/GR/GCE),成功地被用于測定異煙肼。通過掃描電鏡對此修飾電極的表面形貌進(jìn)行了表征,Co_3O_4納米粒子和GR能夠很好地修飾在玻碳電極表面。采用差分脈沖法(DPV)優(yōu)化了異煙肼的測定條件,在最佳條件下,線性關(guān)系范圍為0.5~160μM,最低檢出限為0.17μM(S/N=3),實際藥物和血清中的回收率良好,相對標(biāo)準(zhǔn)偏差均小于5%。該方法方便可行,結(jié)果滿意,重復(fù)性好,實用性強(qiáng)。實驗表明,相比于裸電極,此修飾電極獲得了更好的電化學(xué)性能,可顯著提高對異煙肼的電催化活性。2、在上述工作的基礎(chǔ)上,以GR為基底,利用半胱氨酸氧化為磺基丙氨酸(Cysteic acid,CA)電化學(xué)反應(yīng)及其在GR表面的吸附和聚合,制得石墨烯-磺基丙氨酸復(fù)合膜修飾玻碳電極(GR/CA/GCE),并應(yīng)用于異煙肼含量的測定。在最佳條件下,線性關(guān)系范圍擴(kuò)大為0.1~200μM,最低檢出限僅為0.03μM(S/N=3),具有很高的靈敏度和選擇性。該方法用于藥品中異煙肼的定量分析獲得了滿意的結(jié)果。3、運(yùn)用一種溫和而新穎的電化學(xué)技術(shù)制備了GR和納米氧化鋅(ZnO)復(fù)合物修飾電極(ZnO/GR/GCE)。實驗表明,復(fù)合物修飾電極具有優(yōu)異的電化學(xué)性能;與此同時,該復(fù)合物作為電極的增敏材料,氧氟沙星在該電極上的電催化性能得到了顯著的提高。在最佳測定條件下,氧氟沙星的線性范圍分1~100μM,對應(yīng)的檢測限和靈敏度分別為1.7μM和1399.86μA mM-1 cm-2。同時,該修飾電極在藥品氧氟沙星的檢測中表現(xiàn)出令人滿意的應(yīng)用結(jié)果。4、利用多壁碳納米管(MWCNTs)的優(yōu)良性能,構(gòu)建了MWCNTs和維生素B12(VB12)復(fù)合膜修飾玻碳電極測定對羥基苯乙酮(p-Hyd)的電化學(xué)分析方法。傅里葉變換紅外光譜和電化學(xué)阻抗譜實驗表明,MWCNTs和VB12已經(jīng)成功地修飾在玻碳電極表面。通過優(yōu)化,選擇pH 6.0的磷酸鹽緩沖溶液、VB12電聚合15圈作為最佳優(yōu)化條件,以方波伏安法檢測p-Hyd。實驗結(jié)果表明,與聚鉻黑T修飾電極相比,p-Hyd的氧化電位負(fù)移了0.04 V,雖檢測限沒有改變,但在0.5~20μM和20~200μM范圍內(nèi)均有較好的線性關(guān)系。5、建立了聚鉻黑T修飾玻碳電極方波伏安法測定p-Hyd的電化學(xué)方法。運(yùn)用循環(huán)伏安法在含有0.5 mM鉻黑T的0.1 M NaOH溶液中制備聚鉻黑T膜,并使用掃描電鏡、紅外光譜、電化學(xué)阻抗等技術(shù)進(jìn)行了表征。在優(yōu)化的實驗條件下,p-Hyd在0.91V(vs SCE)處的峰電流與其濃度在1~160μM范圍內(nèi)呈現(xiàn)良好的線性關(guān)系,檢測限達(dá)到0.15μM(S/N=3),相對標(biāo)準(zhǔn)偏差小于2%。該方法簡單易行,具有良好的重現(xiàn)性和穩(wěn)定性。
[Abstract]:Drug analysis is an important branch of analytical chemistry. With the development of pharmacy, drug analysis has gradually become an independent subject. Modern drug analysis has been greatly expanded in both analytical and analytical techniques. As one of the analytical techniques, electrochemical analysis has been widely used in the domain of drug analysis. Because of its advantages of high sensitivity, quick response, good selectivity and simple operation, the electrochemical analysis has injected new vitality into the application of electrochemical analysis in the analysis of drugs. As the research of electrochemical analysis is deepening, the electrochemical analysis is becoming more and more widely used in scientific research and production. And it plays an important role in the research and development of new drugs and drug production. This paper mainly studies the preparation of a new carbon based nanocomposite modified electrode, and explores the electrochemical behavior and electrode reaction mechanism of different drugs on the modified electrode. Thus a sensitive, simple and accurate method for quantitative analysis of drugs is established. The main contents are summarized as follows: 1, a new type of nano composite electrode (Co_3O_4/GR/GCE) was prepared by electrodeposition of metal oxide four oxidation three cobalt (Co_3O_4) / graphene (GR) nanomaterials on the surface of glassy carbon electrode, which was successfully used for the determination of isoniazid. The Co_3O_4 nanoparticles and GR can be well modified on the surface of the glassy carbon electrode. The determination conditions of isoniazid are optimized by differential pulse (DPV). Under the optimum conditions, the linear range is 0.5~160 mu M, the minimum detection limit is 0.17 u M (S/N=3). The recovery rate in the actual drug and serum is good, and the relative standard deviation is less than 5%.. The method is convenient, satisfactory, reproducible and practical. The experiment shows that the electrochemical performance of the modified electrode is better than that of the bare electrode. The electrocatalytic activity of isoniazid can be improved significantly by.2. On the basis of the above work, GR is used as the base and the electrochemistry of Cysteic acid (CA) is oxidized by cysteine. The graphene sulfonyl alanine composite membrane modified glassy carbon electrode (GR/CA/GCE) was prepared by the study of the reaction and its adsorption and polymerization on the GR surface. It was applied to the determination of isoniazid content. Under the optimum conditions, the linear range was expanded to 0.1~200 mu M, the minimum detection limit was only 0.03 Mu M (S/N =3), with high sensitivity and selectivity. The method was used in this method. The quantitative analysis of isoniazid in the drug obtained a satisfactory result.3. GR and nano Zinc Oxide (ZnO) composite modified electrode (ZnO/GR/GCE) was prepared by a mild and novel electrochemical technique. The experiment showed that the composite modified electrode had excellent electrochemical performance. At the same time, the complex was used as an electrode sensitizing material, oxygen fluoride. The electrocatalytic performance of floxacin on this electrode has been greatly improved. Under the optimal determination conditions, the linear range of ofloxacin is 1~100 mu M, the corresponding detection limits and sensitivity are 1.7 mu M and 1399.86 A mM-1 cm-2. respectively. The modified electrode shows a satisfactory application result in the detection of ofloxacin, which is used for the use of.4. The excellent properties of multi wall carbon nanotube (MWCNTs) were obtained. The electrochemical analysis method of MWCNTs and vitamin B12 (VB12) composite membrane modified glassy carbon electrode for the determination of hydroxyacetophenone (p-Hyd) was constructed. The Fourier transform infrared spectroscopy and electrochemical impedance spectroscopy showed that MWCNTs and VB12 had been successfully modified on the surface of the glassy carbon electrode. The selection of pH by optimization was made. 6 phosphate buffer solution and VB12 electropolymerization 15 ring are the best optimization conditions. The test results of p-Hyd. test by square wave voltammetry show that the oxidation potential of p-Hyd is negatively shifted 0.04 V compared with the polychrome black T modified electrode. Although the detection limit is not changed, there is a good linear relationship between 0.5~20 mu M and 20~200 Muu enclosure, and the polychrome black T is established. The electrochemical method for the determination of p-Hyd by modified glassy carbon electrode by square wave voltammetry. The polychrome black T film was prepared by cyclic voltammetry in 0.1 M NaOH solution containing 0.5 mM chromium black T and characterized by scanning electron microscopy, infrared spectroscopy and electrochemical impedance techniques. The peak current and concentration of p-Hyd at 0.91V (vs SCE) at the optimum experimental conditions A good linear relationship is presented in the range of 1~160 mu M, the detection limit is 0.15 mu M (S/N=3), and the relative standard deviation is less than 2%.. The method is simple and easy, and has good reproducibility and stability.

【學(xué)位授予單位】：上海大學(xué)
【學(xué)位級別】：博士
【學(xué)位授予年份】：2016
【分類號】：O657.1;R917

【參考文獻(xiàn)】

相關(guān)期刊論文 前1條

1 葉娉;萬麗;周立;王敏;王凌;;HPLC法測定濱蒿中對羥基苯乙酮[J];中草藥;2009年04期

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本文編號：1818685