新型碳纳米复合材料在大环内酯类和酚类药物电化学检测中的应用

发布时间：2018-01-16 05:10

本文关键词：新型碳纳米复合材料在大环内酯类和酚类药物电化学检测中的应用　出处：《江西科技师范大学》2015年硕士论文　论文类型：学位论文

【摘要】：在药物分析领域,其传统的分析方法主要为生物分析法、电泳法、荧光光谱法、紫外光谱法、高效液相色谱法、气相色谱法、色谱与质谱联用法等,这些方法已经成为药物分析领域中的主流,在检测药物有效成分以及药物残留等方面得到了广泛地应用。然而,尽管这些技术在检测灵敏度等方面得到了广泛的认可,但是由于该类方法在进行分析之前往往需要对样品进行预处理,在分析检测的过程中需要专业的技术人员进行操作,以及本身仪器价格昂贵、体积较大等原因,使得这一类方法很难实现样品的在线检测与分析。而电化学传感器由于其具有简便、快捷、灵敏度高而且能够实现对分析物的在线检测与分析越来越受到人们的关注。因此,电化学传感在药物分析中的优越性也越来越得到人们的认可。本论文工作在综合文献报道的基础上,针对多壁碳纳米管(MWCNTs)和氧化石墨烯(GO)拥有高的比表面积、独特空间结构和易于功能修饰等特点,紧紧围绕碳纳米管和氧化石墨烯这两种碳纳米增强的复合物构建了一系列的大环内酯类和酚类药物电化学传感器,具体内容如下：(1)利用简单的超声的方法制备了氧化石墨烯-多壁碳纳米管(GO-MWCNTs)复合材料。通过透射电镜、拉曼光谱、红外光谱、紫外光谱、电化学阻抗等手段对材料进行了表征,发现MWCNTs可以与GO进行很好地结合,并且GO会吸附到MWCNTs的表面形成项链状的形貌结构。该复合材料进一步被应用于大环内酯类药物-阿奇霉素电化学传感器的构建。电化学数据显示,与裸玻碳电极、GO以及MWCNTs修饰的电极相比,GO-MWCNTs修饰的电极对阿奇霉素显示出较大的氧化峰电流。在最佳条件下氧化峰的大小与被测阿奇霉素的浓度成正比,且其线性范围是0.1～10μM,最低检测限是0.07μM。为了进一步探索其在实际样品中的应用,GO-MWCNTs修饰电极构建的传感平台成功被用于阿奇霉素药片中阿奇霉素含量的测定,并取得了满意的效果。(2)通过界面聚合的方法制备了氧化石墨烯／聚(3,4-乙撑二氧噻吩)(GO/PEDOT)复合材料,利用透射电镜、红外光谱、拉曼光谱、电化学阻抗等手段对材料进行了表征,结果证实PEDOT可以与GO很好地复合在一起。最后将GO/PEDOT复合材料修饰的电极应用于芦丁电化学传感器的构建,实现了对芦丁的分析检测,并进一步提出了芦丁可能的氧化机理。在最佳条件下,电极对芦丁氧化峰的电流大小与芦丁的浓度呈线性相关关系,其检测的线性范围是0.004～60μM,其最低检测限可以达到0.00125μM,而且该电化学传感器实现了实际芦丁药品中芦丁含量的分析与检测。(3)与GO相比,基于MWCNTs纳米材料修饰的电极对某些药物分子可以显示出更强的催化作用,因此利用界面聚合的方法同时制备了多壁碳纳米管／聚(3,4-乙撑二氧噻吩)(MWCNTs/PEDOT)复合材料,利用透射电镜、红外光谱、拉曼光谱、电化学阻抗以及电量—时间曲线等手段对材料进行了表征,结果表明PEDOT膜可以成功地吸附在MWCNTs的表面。最后,将MWCNTs/PEDOT复合材料应用于厚朴酚电化学传感器的构建。通过对检测时实验条件进行优化,确立了该电化学传感器在pH值等于7.0时对厚朴酚具有最佳的检测效果,其检测的线性范围是0.01～25μM,最低检测限可以达到0.003μM,该电化学传感器可以应用于厚朴提取物中厚朴酚含量的测定。(4)利用一步电化学的方法,将具有纳米结构的GO-MWCNTs作为掺杂剂导入PEDOT的基体中,制备了(GO-MWCNTs/PEDOT复合材料,并利用该复合材料构建了己烯雌酚电化学传感器。通过对构建的该电化学传感器实验参数的优化可知,当缓冲溶液的pH值为7.0,富集时间为120s时,该电化学传感器对己烯雌酚具有最佳的检测效果,其检测的线性范围是0.01～20μM,最低检测下限为0.003μM,而且该电化学传感器可以应用于己烯雌酚片中己烯雌酚的含量分析与检测。
[Abstract]:In the field of drug analysis, the traditional analysis method for biological analysis, electrophoresis, fluorescence spectroscopy, UV spectroscopy, high-performance liquid chromatography, gas chromatography, gas chromatography and mass spectrometry, these methods have become the mainstream in the field of drug analysis, has been widely used in detection of the active ingredient of the drug and drug residue. However, although these techniques in detection sensitivity have been widely recognized, but because this kind of method needs sample pretreatment often before analysis, in the process of analysis of professional and technical personnel to operate, and its equipment is expensive, volume big and other reasons, makes this method very difficult to realize the on-line detection and analysis of samples. And the electrochemical sensor because of its simple, fast, high sensitivity and can realize the analysis of matter The online detection and analysis has attracted more and more attention. Therefore, electrochemical sensing superiority in pharmaceutical analysis is more and more recognized by people. The work in this thesis is based on the literatures on the multi walled carbon nanotubes (MWCNTs) and graphene oxide (GO) has high specific surface area. The unique spatial structure and easy modification and other characteristics, closely around the complexes of carbon nanotubes and graphene oxide of the two carbon nano enhanced constructed a series of macrolide drugs and phenol electrochemical sensor, the specific contents are as follows: (1) graphene oxide / multi walled carbon nanotubes were synthesized by a simple method the ultrasound system (GO-MWCNTs) composite material. By transmission electron microscopy, Raman spectroscopy, infrared spectroscopy, UV spectroscopy, the materials were characterized by electrochemical impedance method, found that MWCNTs can be well combined with GO and GO. Will be adsorbed to the morphology and structure formation of necklace like the surface of the MWCNTs. The composite material is further applied to macrolide drug azithromycin electrochemical sensor was constructed. The electrochemical data show that compared with the bare glassy carbon electrode, GO electrode and MWCNTs modified electrode, GO-MWCNTs modified to azithromycin showed the oxidation peak current in larger. The concentration of the oxidation peak under optimum conditions and measured the size of azithromycin is proportional, and the linear range is 0.1 ~ 10 M, the minimum detection limit is 0.07 M. in order to further explore its application in actual sample, sensing platform to construct a GO-MWCNTs modified electrode was successfully used for the determination of azithromycin tablets and azithromycin. Have achieved satisfactory results. (2) by interfacial polymerization method to prepare graphene oxide / poly (ethylene oxide 3,4- two thiophene) (GO/PEDOT) composite materials, using transmission power Mirror, infrared spectroscopy, Raman spectroscopy, the materials were characterized by electrochemical impedance method, the results demonstrated that PEDOT and GO can be well combined together. Finally build the GO/PEDOT composite modified electrode applied to rutin electrochemical sensor, realizes the analysis of detection of rutin, and further puts forward the mechanism of oxidation of rutin may. Under the optimum conditions, a linear correlation relationship between the concentration of rutin oxidation peak current of the electrode size and rutin, 0.004 to the detection linear range is 60 M, the lowest detection limit can reach 0.00125 M, and the electrochemical sensor realizes the detection and analysis of the actual content of Rutin in drug (rutin. 3) compared with GO, MWCNTs modified electrodes of nanometer materials can be of some drug molecules showed stronger catalysis based on the method of interfacial polymerization and preparation of multi walled carbon nanotubes were prepared Poly (ethylene / 3,4- two oxygen thiophene) (MWCNTs/PEDOT) composite materials, using transmission electron microscopy, infrared spectroscopy, Raman spectroscopy, the materials were characterized by electrochemical impedance and power time curve method, the results show that the PEDOT film can be successfully adsorbed on the surface of MWCNTs. Finally, the construction of MWCNTs/PEDOT composite used in Magnolia officinalis the phenol electrochemical sensor. Based on the experimental conditions of detection were optimized, established the electrochemical sensor in pH with value equal to the optimal detection performance of magnolol from 0.01 to 7, the linear range of detection is 25 M, the lowest detection limit can reach 0.003 M, the electrochemical sensor can be applied to the determination of magnolol the content of magnolia bark extract in. (4) using the method of one step electrochemical, with nano GO-MWCNTs as matrix dopants into PEDOT in the preparation of the composite material (GO-MWCNTs/PEDOT And, using the composite material constructed Diethylstibestrol electrochemical sensor. By optimizing the experimental parameters of the electrochemical sensor constructed, when the pH value of buffer solution was 7, the accumulation time is 120s, the electrochemical sensor has the best detection effect of diethylstilbestrol, 0.01 to the linear range of detection 20 M, the minimum detection limit of 0.003 M, content analysis and detection and the electrochemical sensor can be applied to Diethylstilbestrol Tablets in diethylstilbestrol.

【学位授予单位】：江西科技师范大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：O657.1;TB33

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