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Analytical Application Of Flow Injection Chemiluminescence In Pharmaceutical And Metal Ion Analysis

Posted on:2010-10-09Degree:MasterType:Thesis
Country:ChinaCandidate:J ShenFull Text:PDF
GTID:2144360275452015Subject:Environmental Science
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Chemiluminescence(CL) analysis is a method based on the light emission produced from the chemical reactions.When coupled with flow injection,it has the advantages of high sensitivity,wide linear range,simple instrumentation,easy operation, rapid analysis,easily automation,etc;therefore,this method has been widely used in the analysis of trace chemical substances.The paper mainly refers to the analytical application of flow injection chemiluminescence in pharmaceutical and metal ion analysis and consists of two parts including summary and the research works.The first part briefly reviews the basic principles of chemiluminescence,the research development,the coupled technology and its actuality of the analytical application in pharmaceutical and metal ion analysis.It explains the meaning and purpose of the research works.The second part is research works,which include four chemiluminescence systems. Based on the reaction systems of potassium permanganate-Rh6G,luminol-potassium ferricyanide and luminol-potassium permanganate and post-chemiluminescence systems, the new methods for the determination of protocatechuic aldehyde in Fufang Danshen injection samples,ferulic acid in Fufang Danggui injection samples,neomycin in neomycin tablets and cadmium ion in water samples have been developed.1.Determination of protocatechuic aldehyde using the KMnO4- Rh6G systemIn acid medium,the reaction of KMnO4 and protocatechuic aldehyde has faint luminescence;however,their CL intensity could be enhanced in the presence of rhodamine-6G.Based on this phenomenon,a flow injection chemiluminescence method for the determination of protocatechuic aldehyde with simplicity,rapidness and high sensitivity was firstly described.The increase of CL emission was correlated with protocatechuic aldehyde concentration in the range from 5.0×10-7 mol/L -1.0×10-4 mol/L.The detection limit was 1.3×10-8mol/L and the relative standard deviation for the determination of 2.0×10-6 mol/L protocatechuic aldehyde was 1.2%(n = 9).The method has been successfully applied to the determination of protocatechuic aldehyde of Fufang Danshen injection sample and the recoveries are between 101.7%and 107.5%.The chemiluminescence mechanism of the system was discussed.2.Determination of ferulic acid by the luminol- K3Fe(CN)6 systemA flow injection chemiluminescence inhibition method for the determination of ferulic acid was firstly described based on the phenomenon that the chemiluminescence intensity of the luminol- K3Fe(CN)6 system could be inhibited in the presence of ferulic acid.Under the optimum conditions,the decrease of chemiluminescence emission was linear with ferulie acid concentration in the range from 4.0×10-7 to 4.0×10-6 mol/L and the detection limit for ferulic acid was 2.4×10-7 mol/L.The relative standard deviation was 1.4%for 1.0×10-6 mol/L ferulic acid(n = 9).The method has been applied to the determination of ferulic acid of Fufang Danggui injection samples with satisfactory results.Furthermore,the inhibition mechanism was discussed. 3.Determination of neomycin by post-chemiluminescence of luminol- K3Fe(CN)6 systemA new chemiluminescence reaction,called post-chemiluminescence,was found when neomycin was injected into the reaction mixture of alkaline luminal and potassium ferricyanide.The reaction conditions were optimized and a new chemiluminescence method for the determination of neomycin with flow injection technique based on the post-chemiluminescence reaction was developed.The linear range is 1.0×10-5-1.0×10-3 mol/L,and the detection limit is 2.9×10-6 mol/L.The relative standard deviation for the determination of 1.0×10-5 mol/L neomycin is 3.6% (n = 9).The method has been successfully applied to the determination of neomycin in neomycin tablets.4.Determination of cadmium ion by post-chemiluminescence of luminol- KMnO4 systemIt was found that a new chemiluminescence reaction occured and very strong chemiluminescence signal could be detected when the cadmium ion solution was injected into the reaction mixture of alkaline luminol with potassium permanganate, which has finished the chemiluminescence reaction.Under the optimum conditions,the increase of CL emission was correlated with the concentration of cadmium in the range from 8.0×10-7-1.0×10-4 mol / L.The detection limit was 5.2×10-8mol/L,and the relative standard deviation was 1.1%for 1.0×10-6mol/L cadmium ion(n = 9).The method has been successfully applied to the determination of the cadmium concentration in synthetic water samples.
Keywords/Search Tags:Chemiluminescence, Flow injection, Pharmaceutical analysis, Cadmium ion, Post-chemiluminescence
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