本文關(guān)鍵詞： 碳糊電極 氧化鉭 氧化鈮 殼聚糖 同時(shí)檢測(cè) 白楊素 黃芩素 黃芩苷　出處：《鄭州大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

【摘要】：碳糊電極自從1958年問(wèn)世以來(lái),就因具有易被修飾、電位窗寬、表面可重復(fù)利用率高等獨(dú)特的優(yōu)點(diǎn)在電化學(xué)領(lǐng)域廣受歡迎。其中碳糊電極最有價(jià)值的特點(diǎn)就是易被各種水溶性或非水溶性材料修飾。近年來(lái)的發(fā)展表明,通過(guò)金屬氧化物粒子修飾碳糊電極受到越來(lái)越多電分析工作者的青睞,以綠色、簡(jiǎn)單易行、靈敏高效等優(yōu)點(diǎn)著稱,通過(guò)構(gòu)筑不同的金屬氧化物粒子修飾碳糊電極,輔以電活化、沉積等一些手段,進(jìn)而篩選最優(yōu)構(gòu)筑條件,發(fā)揮最大性能,從而實(shí)現(xiàn)對(duì)藥物分子的靈敏檢測(cè),最終用于對(duì)生物體的的實(shí)時(shí)監(jiān)測(cè),研究藥物在生物體內(nèi)的轉(zhuǎn)化關(guān)系和速率。基于此,我們借助具有高催化性能的過(guò)渡金屬氧化物粒子Ta_2O_5和Nb_2O_5及殼聚糖粉末修飾碳糊電極,完成了一系列應(yīng)用。主要工作如下:(1)首先基于電化學(xué)活化Ta_2O_5粒子修飾碳糊電極(EA-Ta_2O_5-CPE)制備了一種新穎的伏安傳感器。采用掃描電鏡(SEM)、X-射線衍射光譜(XRD)、循環(huán)伏安法(CV)和電化學(xué)阻抗譜(EIS)對(duì)電極的表面結(jié)構(gòu)形態(tài)和傳感性能進(jìn)行了表征,實(shí)驗(yàn)數(shù)據(jù)表明該傳感器有卓越的電催化性能,對(duì)白楊素有良好的伏安響應(yīng)。隨后,采用線性掃描伏安法建立了白楊素的標(biāo)準(zhǔn)曲線,其響應(yīng)的線性范圍為5.0×10~(-7) mol L~(-1)-7.0×10~(-6) mol L~(-1),檢出限(S/N=3)為2.0×10~(-8) mol L~(-1)。最后,將建立的方法成功地應(yīng)用于白楊素膠囊和中草藥木蝴蝶中白楊素的含量的測(cè)定,結(jié)果滿意。(2)為進(jìn)一步提高電極的穩(wěn)定性和靈敏度,采用直接混合法制備了殼聚糖(CTS)、Ta_2O_5粒子修飾的碳糊電極(Ta_2O_5-CTS-CPE)。通過(guò)對(duì)電極的組成和操作條件進(jìn)行系統(tǒng)優(yōu)化實(shí)現(xiàn)了對(duì)白楊素和黃芩素的同時(shí)檢測(cè),構(gòu)筑電極對(duì)白楊素和黃芩素的線性響應(yīng)范圍是8.0×10~(-8) mol L~(-1)-4.0×10~(-6) mol L~(-1),檢出限(S/N=3)分別為3.0×10~(-8) mol L~(-1)和5.0×10~(-8) mol L~(-1)。根據(jù)實(shí)驗(yàn)數(shù)據(jù),給出了合理的白楊素和黃芩素在目標(biāo)電極上的反應(yīng)機(jī)理。同時(shí),測(cè)定了中草藥木蝴蝶活性成分中白楊素和黃芩素的含量,得到了令人滿意的結(jié)果。(3)在之前研究的基礎(chǔ)上,構(gòu)筑了雙金屬氧化物Ta_2O_5-Nb_2O_5復(fù)合殼聚糖修飾碳糊電極(Ta_2O_5-Nb_2O_5@CTS-CPE)。Ta_2O_5-Nb_2O_5@CTS-CPE對(duì)黃芩素和黃芩苷都有靈敏的響應(yīng)且可以實(shí)現(xiàn)對(duì)二者的同時(shí)檢測(cè)。在最佳條件下,采用差分脈沖法建立了黃芩素和黃芩苷的標(biāo)準(zhǔn)曲線,線性范圍為8.0×10~(-8) mol L~(-1)至8.0×10~(-6) mol L~(-1),檢出限(S/N=3)分別為5.0×10~(-8) mol L~(-1)和3.0×10~(-8) mol L~(-1)。最后,目標(biāo)電極成功應(yīng)用于探究生物體內(nèi)黃芩苷的水解過(guò)程和測(cè)定中草藥黃芩樣品中黃芩苷和黃芩素的含量。
[Abstract]:Since the carbon paste electrode was introduced in 1958, it has been easy to be modified and has wide potential window. The unique advantages of high surface repeatability are popular in the electrochemical field. The most valuable characteristic of carbon paste electrode is that it is easy to be modified by a variety of water-soluble or insoluble materials. Recent development shows that carbon paste electrode is easy to be modified by various water-soluble or insoluble materials. Carbon paste electrode modified by metal oxide particles is favored by more and more electrical analysts. It is famous for its advantages such as green, simple, sensitive and efficient. By constructing different metal oxide particles modified carbon paste electrodes, with some means such as electric activation, deposition, and so on, we can select the best construction conditions and give full play to the maximum performance, so as to achieve the sensitive detection of drug molecules. Finally, it is used to monitor the organism in real time, and to study the transformation relationship and rate of drugs in organism. Based on this. Carbon paste electrodes were modified with transition metal oxide particles (Ta_2O_5 and Nb_2O_5) and chitosan powder with high catalytic performance. A series of applications have been completed. The main work is as follows: (1) first of all, the carbon paste electrode modified by Ta_2O_5 particles based on electrochemical activation is used to modify the carbon paste electrode. A novel voltammetry sensor was prepared by scanning electron microscopy (SEM). The surface morphology and sensing properties of the electrode were characterized by X-ray diffraction (XRD), cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The experimental data show that the sensor has excellent electrocatalytic performance and good voltammetric response to salicylate. Subsequently, the standard curve of the sensor is established by linear scanning voltammetry. The linear range of its response is 5.0 脳 10 ~ (-7) mol / L ~ (-1) -7.0 脳 10 ~ (-1) mol / L ~ (-1)). The detection limit of S / N ~ (3) is 2.0 脳 10 ~ (-8) mol. The established method has been successfully applied to the determination of the content of aspen in poplar capsules and Chinese herbal medicine. The results are satisfactory. 2) to further improve the stability and sensitivity of the electrode. Chitosan CTS were prepared by direct mixing method. The carbon paste electrode modified by Ta_2O_5 particles was used for the simultaneous detection of Baicalin and baicalin by systematically optimizing the composition and operating conditions of the electrode. The linear response range of the constructed electrode to salicylate and baicalein is 8.0 脳 10 ~ (-8) mol / L ~ (-1) -4.0 脳 10 ~ (-1) mol / L ~ (-1)). The detection limits of S / N ~ (3) were 3.0 脳 10 ~ (-8) mol / L ~ (-1) and 5.0 脳 10 ~ (-8) mol / L ~ (-1), respectively. The reaction mechanism of Baicalin and paeicalin on the target electrode was given. Meanwhile, the contents of salicylin and baicalin in the active components of Chinese herbal medicine were determined. Satisfactory results have been obtained on the basis of previous studies. The carbon paste electrode modified by bimetallic oxide Ta_2O_5-Nb_2O_5 was constructed. Tasp _ 2O5-Nb2O5-CTS-CPE has a sensitive response to both baicalin and baicalin and can be detected simultaneously under the best conditions. The standard curves of baicalin and baicalin were established by differential pulse method. The linear range is 8.0 脳 10 ~ (-8) mol / L ~ (-1) to 8.0 脳 10 ~ (-6) mol / L ~ (-1)). The detection limits of S / N ~ (3) were 5.0 脳 10 ~ (-8) mol / L ~ (-1) and 3.0 脳 10 ~ (-8) mol / L ~ (-1) respectively. The target electrode was successfully used to study the hydrolysis process of baicalin and to determine the content of baicalin and baicalin in the samples of Scutellaria baicalensis.
【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】：2017
【分類號(hào)】：R917;O657.1

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