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Study Of Fluorescent Spectro Electrochemistry Analysis In The Determination Of Several Drugs

Posted on:2011-08-31Degree:MasterType:Thesis
Country:ChinaCandidate:Y LiFull Text:PDF
GTID:2154360308975956Subject:Analytical Chemistry
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As one of the important pharmaceutical analysis methods, the fluorescence analysis has developed fast in recently years and been widely used in drug analysis because of high sensitivity and good selectivity. Many pharmaceutical molecules could have strong fluorescence after being oxidized or reduced although they have no or weak native fluorescence characteristics. In this paper, a simple and sensitive spectro- electrochemistry method has been described by combining fluoremetry and eletrolysis to study on the concentration determination of carbamazepin, reserpine, epinephrine and vitamin K3.This paper consists of two parts, which are literature review and research report, respectively.In the first part (Chapter 1), literature review, the classification and the progress of the fluoremetric analysis are reviewed, and the applications of the methods mentioned are introduced with examples.The second part, research report, consists of five chapters.In Chapter 2, the main instruments, the reagents used in the experiment and the approaches of experiment are introduced.In Chapter 3, a simple and sensitive electrolysis-fluorescence method has been developed by combining electrolysis and fluoremetry for the determination of CBZ. This method is based on that CBZ can be oxidated by electrolysis at a Pt electrode,and the product has a characteristic fluorescence at 478nm with excitation wavelength at 247 nm. Under the optimum conditions, the fluorescence intensity was proportional to the concentration of CBZ over the range from 1.00×10-8 mol/L to 1.00×10-6 mol/L, with a 2.13×10-9 mol/L detection limit. The result is satisfactory for the determination of CBZ in tablets.In Chapter 4, reserpine was electro-oxidize at a platinum electrode,and its product has a characteristic fluorescence at 495 nm with excitation wavelength at 385 nm. Under the optimum conditions, the fluorescent intensity of the electrolyzed product was proportional to the concentration of reserpine over the range from 6.00×10?8 to 2.00×10?6 and 2.00×10?6 to 8.00×10?5 mol/L, with a 3.90×10?8 mol/L detection limit. The relative standard deviation was less than 2.33% (n=7) and the recovery was in the range of 96.0~104% for the determination of reserpine in pharmaceutical samples.In Chapter 5, the spectroelectrochemistry was employed for the determination of epinephrine. This method is based on that Ep can be electro-oxidize at a platinum electrode,and its product has a characteristic fluorescence at 490 nm with excitation wavelength at 328 nm. Under the optimum conditions, the electrogenerated fluorescent intensity was proportional to the concentration of epinephrine over the range from 2.00×10?7 to1.00×10?6 mol/L and 1.00×10?6 to 4.00×10?5 mol/L, with a 6.70×10?8 mol/L detection limit The relative standard deviation was less than 1.88% (n=5) and the recovery was in the range of 89.6~109% for the determination of epinephrine in pharmaceutical samples.The last chapter described the fluorescent spectroelectrochemistry method for determination of vitamin K3 which is based on that vitamin K3 was reduced at a glassy carbon electrode, and its product with characteristic fluorescence at 420 nm was determined with excitation wavelength at 309 nm. Under optimizing the electrochemical reaction conditions and fluorescent experiment parameters, the fluorescence intensity was proportional to the concentration of vitamin K3 over the range from 2.00×10-8 mol/L to 1.60×10-5 mol/L, and detection limit was estimated to be 3.08×10?8mol/ L . The relative standard deviation was less than 4.3 % (n=5) and the recovery was in the range of 88.5~103% for the determination of vitamin K3 in pharmaceutical preparations.
Keywords/Search Tags:fluorescent, spectroelectrochemistry, carbamazipine, resepine, epinephrine vitamin K3
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