【作者】 张婧；

【导师】 康维钧；

【作者基本信息】 河北医科大学 ， 卫生毒理学， 2010， 硕士

【摘要】 流动注射技术具有灵敏度高,线性范围宽,分析速度快及仪器设备相对简单等优点,可广泛应用于生命科学、环境科学和临床医学等领域。本研究室前期工作发现,在碱性介质中,Ag(III)配合物可氧化鲁米诺产生稳定的化学发光信号,某些物质能显著增强鲁米诺-Ag(III)体系的化学发光,且发光强度与物质浓度在一定范围内呈良好的线性关系。基于此,本文将Ag(III)-鲁米诺化学发光新体系结合流动注射技术,建立了测定芦丁,尿酸和去甲肾上腺素三种物质的新方法,并通过固相萃取等方法实现样品的提取,可有效的消除某些干扰杂质,简化了样品预处理过程,其操作过程简便,结果灵敏可靠。目的:建立测定芦丁,尿酸和去甲肾上腺素的流动注射化学发光新方法。方法:在碱性条件下,Ag(III)可以氧化鲁米诺产生稳定的化学发光信号,芦丁、尿酸和去甲肾上腺素能显著增强Ag(III)-鲁米诺体系的化学发光作用,且发光强度与样品的浓度在一定范围内呈良好的线性关系。通过对鲁米诺浓度,Ag(III)溶液浓度等一系列发光条件进行优化,并绘制标准曲线,将处理过的样品进行测定。结果:1流动注射-化学发光法测定芦丁的最低检出限为4.0×10-7g/L。线性范围为2.0×10-5-2.0×10-3g/L,回归方程为△I=4.46×108C+445,线性相关系数r=0.9931。对2.0×10-4g/L的芦丁连续进行平行测定11次,相对标准偏差为0.937%,加标回收率在90.0%-100.0%之间。2流动注射-化学发光法测定尿酸的最低检出限为2.0×10-10mol/L。线性范围为2.0×10-9-2.0×10-7mol/L,回归方程为△I=1.41×1011C+502,相关系数r=0.9968。对5.0×10-8mol/L的尿酸连续进行平行测定9次,相对标准偏差为0.625%,加标回收率在98.0%-100.0%之间。3流动注射化学发光法测定去甲肾上腺素的最低检出限为5.0×10-8mol/L。线性范围为1.0×10-7-1.0×10-5mol/L,回归方程为△I=7.39×108C+120,相关系数r=0.9998。对8.0×10-7mol/L的去甲肾上腺素连续进行平行测定11次,相对标准偏差为0.738%,加标回收率在95.0%-100.0%之间。结论:1流动注射化学发光法测定芦丁、尿酸和去甲肾上腺素,方法简便快捷、准确可靠。2用固相萃取SPE与流动注射化学发光分析方法相结合的检测技术经济、简便、快速、准确更多还原

【Abstract】 Flow injection chemiluminescence have the advantages of high sensitivity,wide linear range,rapid analysis and simple apparatus. It is widely used in the areas of life sciences, environmental science, clinical and physiology. Under alkaline conditions, Ag(III) oxide luminol can produce stable chemiluminescence signal. Some substances can significantly enhance the chemiluminescence, and the chemiluminescence intensity showed a good linear relationship to the concentration in a certain range. In this paper, the novel flow-injection chemiluminescence method was establishment for the determination of rutin, uric acid and norepinephrine combined solid-phase extraction through the extraction of samples. In this study, soild-phase extraction can significantly reduce the solvent usage, simplify sample preparation process and speed up sample processing speed, effectively eliminate the interference of certain impurities. The method is simple, fast, accurate and reliable.Objective:To determine rutin, uric acid and norepinephrine by a novel flow injection chemiluminescence method.Methods:Under alkaline conditions, Ag(III) can produce stable oxidation of luminol chemiluminescence signals. Rutin, uric acid and norepinephrine can enhance the chemiluminescence of the luminol-Ag(III) system, and the chemiluminescent intensity show good linearity to the concentration of the analytes within a certain range. The analytes of the standard preparation into a series of standard solutions done the conditions choice. The conditions for the CL detection for three analytes were systematically investigated. It will be treated samples were determined.Finally, this method has been applied for the determination of three analytes in real sample.Results:1. A method of flow-injection chemiluminescence for determination of rutin was developed.The detection limit was 4.0×10-7g/L,The linear equation of the method was△I=4.46×108C+445, r =0.9931,the recoveries of standard addition was in rang of 90.0%-100.0% .The relative standard deviation was 0.937% for 2.0×10-4g/L of rutin (n=11).2. A method of flow-injection chemiluminescence for determination of uric acid was developed.The detection limit was 2.0×10-10mol/L.The linear equation of the method was△I=1.41×1011C +502, r=0.6698,the recoveries of standard addition was in rang of 98.0%-100.0%, The relative standard deviation was 0.625% for 5.0×10-8mol/L of uric acid (n=9), based on signal-to-noise ratio of 3:1.3. A method of flow-injection chemiluminescence for determination of norepinephrine was developed.The detection limit was 5.0×10-8mol/L.The linear equation of the method was△I=7.39×108C+120, r =0.9998 , the recoveries of standard addition was in rang of 95.0%-100.0%.The relative standard deviation was 0.738% for 8.0×10-7mol/L of norepinephrine(n=11).Conclusions:1. The novel Ag(III)-luminol chemiluminescence system can be applied for the determination of rutin, uric acid and norepinephrine. The method is simple, fast, accurate and reliable.2. Solid-phase extraction and flow injection chemiluminescence detection method combining technical is economic, simple, rapid and accurate.更多还原