硝酸铈铵、核黄素和加替沙星的荧光检测新方法研究

发布时间：2018-03-13 18:20

本文选题：荧光碳点　切入点：硝酸铈铵　出处：《西南大学》2017年硕士论文　论文类型：学位论文

【摘要】：近年来,碳点的合成及应用越来越受人关注。基于碳点尺寸小,低毒性,光稳定性,荧光寿命长和良好的水溶性,使得碳点在环境监测、生物成像、生物分子检测分析及药物传递等领域得到应用。荧光光谱法具有操作简便、试剂用量少、选择性好、灵敏度高等特点,因此,荧光光谱法在环境、医学生物、药物、食品等领域的应用越来越广泛。本文主要研究了碳点的合成及其在水体污染物硝酸铈铵和药物核黄素的荧光光谱检测应用,另外建立了新的荧光光谱法测定药物加替沙星。1.荧光碳点的合成、表征及荧光特性研究以马来酸和乙二胺为前驱体采用水热法一步合成碳点溶液,为去除大颗粒固体杂质将溶液放置于离心机中以8000 r/min的速度离心10 min,将滤液用0.22m(44)水性微孔过滤膜过滤后透析提纯,放于真空干燥箱中干燥得到固体片状碳点。分别取适量固体通过紫外吸收、红外、透射电镜做表征、研究了碳点CDs的荧光性能及pH对碳点的影响。2.荧光光谱法研究CDs-CAN体系及其分析应用以碳点CDs作为荧光探针、硝酸铈铵(CAN)为荧光猝灭剂,建立了简单易操作,高效,选择性较好的荧光光谱法检测CAN。在pH为3.0的缓冲溶液中,CAN能有效地猝灭碳点的荧光。在优化条件下,CAN浓度在4.0-140mg mL~(-1)范围内与碳点荧光猝灭值ΔF呈良好的线性关系。检出限为工作曲线下限1.4mg mL~(-1)。考察了常见物质对实验的干扰,结果显示该方法具有良好的选择性。用于水体样品中CAN的测定,回收率为96.2%-101.4%,说明该方法具有较高的准确性,检测结果令人满意。根据温度曲线和UV吸收光谱判断CAN对碳点的猝灭过程属于静态猝灭。3.荧光光谱法研究CDs-VB_2体系及其分析应用以碳点CDs作为能量供体、核黄素作为能量受体,在pH为7.0的缓冲液中加入核黄素,CDs-VB_2体系的荧光强度增强,λ_(ex)=445 nm,而最大发射波长发生红移在520 nm左右。优化条件下,核黄素在3.0-37.5×10-6 mol L~(-1)的浓度范围内与体系荧光增强值ΔF呈现出一定的线性关系。检出限为0.52mM。考察了常见物质及片剂辅料对体系用于测定核黄素的干扰,结果表明其具有良好的选择性。此方法成功地应用于分析测定片剂中核黄素含量。根据紫外吸收和荧光光谱特性探讨了体系反应的机理,表明该荧光强度的增加应归属于荧光共振能量转移机理。4.电荷转移荧光法测定加替沙星氯醌酸(CL)与加替沙星(GFLX)发生电荷转移(CT),该反应中,氯醌酸作为π-电子受体,加替沙星作为电子供体,电荷转移复合物的荧光强度是加替沙星荧光强度的10倍,该复合物在甲醇溶剂里呈现稳定的淡紫色。该荧光光谱法分析检测加替沙星简单,准确,快速,灵敏度高,选择性强,对加替沙星浓度响应线性范围为0.12-10.00mg mL~(-1),具有良好的线性关系R为0.9991,将其应用于加替沙星片剂的含量测定回收率达(100.46±2.04)%。
[Abstract]:In recent years, more and more attention has been paid to the synthesis and application of carbon spots. Due to their small size, low toxicity, light stability, long fluorescence lifetime and good water solubility, carbon spots are monitored in the environment and biologically imaged. Fluorescence spectrometry has been applied in many fields such as biomolecules detection and drug delivery. Fluorescence spectrometry has the advantages of simple operation, less reagent dosage, good selectivity and high sensitivity. Therefore, fluorescence spectrometry is widely used in environment, medical biology, medicine, etc. In this paper, the synthesis of carbon spots and its application in the detection of water pollutants such as cerium ammonium nitrate and riboflavin were studied. In addition, a new fluorescence spectrometric method for the determination of gatifloxacin was established. The synthesis, characterization and fluorescence properties of the fluorescent carbon point were studied. The hydrothermal method was used to synthesize the carbon point solution with maleic acid and ethylenediamine as precursors. In order to remove the large particle solid impurity, the solution was placed in the centrifuge at the speed of 8000 r / min for 10 min. The filtrate was filtered by 0.22 m ~ (44)) water micropore filtration membrane and then purified by dialysis. Solid flake carbon spots were obtained by drying in a vacuum dryer. Appropriate amounts of solids were obtained by UV absorption, infrared and transmission electron microscopy. The fluorescence properties of carbon point CDs and the effect of pH on carbon point were studied. 2. The fluorescence spectrum method was used to study the system of CDs-CAN and its analytical application. The fluorescence quenching agent (CAN) and the carbon point CDs as fluorescence probe were established, which were simple and easy to operate and highly efficient. In the buffer solution of pH 3.0, can can effectively quench the fluorescence of the carbon point. Under the optimized conditions, the concentration of can is in the range of 4.0-140 mg / mL ~ (-1) and has a good linear relationship with the fluorescence quenching value 螖 F of the carbon point. The detection limit was 1.4 mg / mL ~ (-1) of the working curve. The interference of common substances to the experiment was investigated. The results show that the method has good selectivity and has been applied to the determination of CAN in water samples. The recovery rate of this method is 96.2- 101.4, which indicates that the method has high accuracy. According to the temperature curve and UV absorption spectrum, the quenching process of carbon point by CAN belongs to static quenching. 3. Fluorescence spectroscopy was used to study the system of CDs-VB_2 and its analytical application: carbon point CDs as energy donor, riboflavin as energy receptor, riboflavin as energy acceptor, carbon point CDs as energy donor, riboflavin as energy acceptor. The fluorescence intensity of riboflavin CDs-VBs2 system was enhanced by adding riboflavin in buffer solution of pH 7.0, 位 _ (+) _ (+) _ (445nm), and the maximum emission wavelength was shifted to about 520nm. The concentration of riboflavin in the range of 3.0-37.5 脳 10 ~ (-6) mol / L ~ (-1) showed a linear relationship with the fluorescence enhancement value 螖 F of the system. The detection limit was 0.52 mm. The interference of common substances and tablet excipients in the determination of riboflavin in the system was investigated. The method has been successfully applied to the determination of riboflavin in tablets. The mechanism of the reaction is discussed according to the UV absorption and fluorescence spectra. It is suggested that the increase of fluorescence intensity should be attributed to the mechanism of fluorescence resonance energy transfer. 4. The charge transfer reaction between gatifloxacin chloroquinone acid (CLA) and gatifloxacin (GFLX) occurs in this reaction, in which chloroquinonic acid acts as a 蟺 -electron receptor. As an electron donor, gatifloxacin has a fluorescence intensity of 10 times higher than that of gatifloxacin, and the complex presents a stable lavender in methanol solvent. The fluorescence spectrum method is simple and accurate for the determination of gatifloxacin. The linear range for gatifloxacin concentration was 0.12-10.00 mg / mL ~ (-1) with a good linear relationship R = 0.9991. The recovery of gatifloxacin tablets was 100.46 卤2.04m ~ (-1).
【学位授予单位】：西南大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：X832;O657.3;TQ460.72

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