本文選題：熒光碳點　切入點：硝酸鈰銨　出處：《西南大學》2017年碩士論文　論文類型：學位論文

【摘要】：近年來,碳點的合成及應用越來越受人關(guān)注�；谔键c尺寸小,低毒性,光穩(wěn)定性,熒光壽命長和良好的水溶性,使得碳點在環(huán)境監(jiān)測、生物成像、生物分子檢測分析及藥物傳遞等領域得到應用。熒光光譜法具有操作簡便、試劑用量少、選擇性好、靈敏度高等特點,因此,熒光光譜法在環(huán)境、醫(yī)學生物、藥物、食品等領域的應用越來越廣泛。本文主要研究了碳點的合成及其在水體污染物硝酸鈰銨和藥物核黃素的熒光光譜檢測應用,另外建立了新的熒光光譜法測定藥物加替沙星。1.熒光碳點的合成、表征及熒光特性研究以馬來酸和乙二胺為前驅(qū)體采用水熱法一步合成碳點溶液,為去除大顆粒固體雜質(zhì)將溶液放置于離心機中以8000 r/min的速度離心10 min,將濾液用0.22m(44)水性微孔過濾膜過濾后透析提純,放于真空干燥箱中干燥得到固體片狀碳點。分別取適量固體通過紫外吸收、紅外、透射電鏡做表征、研究了碳點CDs的熒光性能及pH對碳點的影響。2.熒光光譜法研究CDs-CAN體系及其分析應用以碳點CDs作為熒光探針、硝酸鈰銨(CAN)為熒光猝滅劑,建立了簡單易操作,高效,選擇性較好的熒光光譜法檢測CAN。在pH為3.0的緩沖溶液中,CAN能有效地猝滅碳點的熒光。在優(yōu)化條件下,CAN濃度在4.0-140mg mL~(-1)范圍內(nèi)與碳點熒光猝滅值ΔF呈良好的線性關(guān)系。檢出限為工作曲線下限1.4mg mL~(-1)。考察了常見物質(zhì)對實驗的干擾,結(jié)果顯示該方法具有良好的選擇性。用于水體樣品中CAN的測定,回收率為96.2%-101.4%,說明該方法具有較高的準確性,檢測結(jié)果令人滿意。根據(jù)溫度曲線和UV吸收光譜判斷CAN對碳點的猝滅過程屬于靜態(tài)猝滅。3.熒光光譜法研究CDs-VB_2體系及其分析應用以碳點CDs作為能量供體、核黃素作為能量受體,在pH為7.0的緩沖液中加入核黃素,CDs-VB_2體系的熒光強度增強,λ_(ex)=445 nm,而最大發(fā)射波長發(fā)生紅移在520 nm左右。優(yōu)化條件下,核黃素在3.0-37.5×10-6 mol L~(-1)的濃度范圍內(nèi)與體系熒光增強值ΔF呈現(xiàn)出一定的線性關(guān)系。檢出限為0.52mM。考察了常見物質(zhì)及片劑輔料對體系用于測定核黃素的干擾,結(jié)果表明其具有良好的選擇性。此方法成功地應用于分析測定片劑中核黃素含量。根據(jù)紫外吸收和熒光光譜特性探討了體系反應的機理,表明該熒光強度的增加應歸屬于熒光共振能量轉(zhuǎn)移機理。4.電荷轉(zhuǎn)移熒光法測定加替沙星氯醌酸(CL)與加替沙星(GFLX)發(fā)生電荷轉(zhuǎn)移(CT),該反應中,氯醌酸作為π-電子受體,加替沙星作為電子供體,電荷轉(zhuǎn)移復合物的熒光強度是加替沙星熒光強度的10倍,該復合物在甲醇溶劑里呈現(xiàn)穩(wěn)定的淡紫色。該熒光光譜法分析檢測加替沙星簡單,準確,快速,靈敏度高,選擇性強,對加替沙星濃度響應線性范圍為0.12-10.00mg mL~(-1),具有良好的線性關(guān)系R為0.9991,將其應用于加替沙星片劑的含量測定回收率達(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 鹵2.04m ~ (-1).
【學位授予單位】：西南大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：X832;O657.3;TQ460.72

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