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Study On Fluorospectrophotometry Of Quinolones And The Residue Analysis

Posted on:2006-12-28Degree:MasterType:Thesis
Country:ChinaCandidate:Y HeFull Text:PDF
GTID:2121360152486092Subject:Environmental Science
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Quinolones is a common used antibiotic in clinic on human and animals. The misunderstanding in antibiotic use led to the practical abuse and the residue in animal original products, as a result of the lack of checkup organization, equipments and perfect determination standard. Thus, it is necessary to set up an exact convenient and high delicate standard. Fluorescence spectrum is molecular emission spectrum of high delicacy, good selectivity, and convenience with a great development in recent years. The analytical methods of Fluorescence spectra on the single or several Quinolones residue have been studied.The experiment showed that intensity of fluorescence of Enoxacin(ENX) in anionic surfactant sodium dodecylsulfate (SDS) micellar system was stronger than Enoxacin alone, which could be set up as a new way to determine the Enoxacin, and the principium of SDS enhancement was discussed. The experiments showed that systematic fluorescence intensity and concentration present good linear relationship, when the concentration of Enoxacin was 2.0×10-74.0×10-6mol/L. The detection limit was 1.4×10-8mol/L. This checkup directly examined the determination of Enoxacin in human urine, with an average recovery within the range of 95.0105.0% and a relative standard deviation of 1.82.5%.And fluorescence characteristics of the complex of terbium(Ⅲ)- Sparfloxacin have been studied. Experiment showed that there was energy transportation betweenSparfloxacin and Tb3+, which enhanced the peak by 50 times. According to this, a method was set up, in which the best term was pH 5.6, Tb3+ concentration of 4.0x10^01/, XexAem=275nm/545nm. The linear range was Ixl0"7mol/L1.5xl0'5 mol/L with the detection limit of l^xlO^mol/L. A new method has been developed for the determination of Sparfloxacin in human urine, and the recovery was within the range of 97-101%, and relative standard deviation 2.4-3.0%. The principium of the complex enhancement has also been studied.The determination of several Quinolones at the same time was the common problem, when the remnant analysis was approaching. The use of multivariate calibration methods and fluorospectrophotometry in Quinolones analysis has been studied taking four branches system of Gatifloxacin, Ofioxacin, Lomefloxacin and Ciprofloxacin jections and the tow branches system of Enrofloxacin and Ciprofloxacin in eggs as examples.The multivariate calibration methods mainly adopted was multiple linear regression(MLR), K metric method(K) and P metric method(P) to prognosticate the concentration of Gatifloxacin, Ofioxacin, Lomefloxacin and Ciprofloxacin in the samples. The experiment showed that MLR was not fine, but K and P with good prognosticated results.The recoveries of the four Quinolones in K were within the range of 93.1-115.0%, 94.7-105.5%, 93.3-116.8%, 91.3-113.7%, and 92.3-113.8%, 97.8-117.5%, 93.3-116.0%, 96.0-118.7% in P. And then the three multivariate calibration methods were adopted in the prognostication of the determination of Enrofloxacin and Ciprofloxacin in the same group of eggs. Prognostication recoveries of the determination of Enrofloxacin in the sample were 85.0%104.5%, 92.0% -125.5%, 91.5%122.5%, and 80.0%114.7%, 95.2%122.4%, 89.6%116.0% of Ciprofloxacin. In the three methods the relative standard deviation was smaller in K and P than MLR. So the result in K and P are better.When multivariate calibration methods was adopted in the prognostication, the large amount of complicated matrix operation was inevitable. So the software of Multivariate Calibration Methods on Photometry Analysis was developed based onMATLAB, which interfaced the data input and output by taking GUI(Graphical User Interfaces) and with a simplified operation.The analysis methods of Fluorescence spectra on the single or several Quinolones residue have been studied. The methods studied here are all of high delicacy, low dictation limit, and low cost, and of practical use. The mechanism of the new methods was also studied.
Keywords/Search Tags:Fluorospectrophotometry, Micellar system, Terbium, Quinolones, Floxacin, Multivariate calibration methods, Multiple linear regression(MLR), K metric method(K), P metric method(P)
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