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Study on the Assay of Pharmaceutical Ingredients with CE-ECL Technology Sensitized by a Modified Electrode
Author: WangWeiFeng
Tutor: MaYongJun
School: Northwest Normal University
Course: Analytical Chemistry
Keywords: Capillary Electrophoresis Chemically modified electrode ECL Bipyridine ruthenium ( II ) Erythromycin ethylsuccinate Azithromycin Roxithromycin Clindamycin Ephedrine Pseudoephedrine Methylephedrine
CLC: R917
Type: Master's thesis
Year: 2011
Downloads: 30
Quote: 0
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Abstract
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The capillary electrophoresis ECL is the fastest developing a new type of separation and analysis technology over the past decade, it integrates a high sensitivity for the efficient separation capability of capillary electrophoresis and electrochemiluminescence detection. ECL analysis of the most widely used light-emitting reagent Ru (bpy) 3 2 sup>, because it has a good water-soluble, chemically stable, redox reversible Features favored oft. CE-ECL technology, the working electrode surface properties of Ru (bpy) 3 2 sup> luminous efficiency a great impact on the working electrode, especially in the separation and analysis of complex sample the antitoxic ability to determine the reliability of detection. PB-Eu modified electrode capable of catalyzing the oxidation process associated pyridine ruthenium, and itself has good stability, and thereby can improve the detection sensitivity and reproducibility of the CE-ECL method. The main contents of the present work is the use of the PB-Eu modified electrode CE-ECL working electrode, macrolides, ephedrine class of drugs for the study object, the separation and analysis of characteristics of the analyte on the electrode to achieve a Determination of several active ingredients of pharmaceutical drugs and traditional Chinese medicine in the content, and the development of the CE-ECL determination of drug - protein binding constant analysis methods. The main research content includes the following four parts: the first review briefly the development and future of the capillary electrophoresis, made a brief introduction to the principle of capillary electrophoresis separation mode, the type of detector; overview of the CE-ECL technology in drug environment and living matter analysis application; introduced the new functional materials applications in the ruthenium bipyridine light-emitting system, and focuses on the application of new materials in the ECL technology, the problems that exist in the development of the analysis system explore and prospects of its development direction. The second chapter of capillary electrophoresis electroluminescent chemiluminescence determination of the erythromycin ethylsuccinate europium ion doped Prussian blue chemically modified platinum electrode couplet electro-catalytic oxidation of Ru (bpy) / erythromycin ethylsuccinate system can significantly enhance the ruthenium bipyridine electroluminescent chemiluminescence intensity, pursuant to which the establishment of the new analysis method of capillary electrophoresis ECL detection of erythromycin ethylsuccinate. Under optimized conditions, the the system luminous intensity and the concentration of erythromycin ethylsuccinate? G / mL ~~ 100? G / mL (R = 0.9993) showed a good linear relationship between the detection limit of 0.25? G / mL ( S / N = 3). Concentration of 10? G / mL of erythromycin ethylsuccinate standard solution continuously measured six times, the luminous intensity and migration time RSD were 2.26% and 0.81%, respectively. This method is rapid, sensitive, accurate, and analytical samples without complicated processing can be directly used in the pharmaceutical and human urine determination of erythromycin ethylsuccinate content. Chapter capillary electrophoresis ECL Determination of azithromycin, roxithromycin and clindamycin and human serum albumin binding constants PB-Eu chemical modified electrode as the working electrode, the establishment of a capillary electrophoresis ECL method sensitive to rapid separation and detection of azithromycin, roxithromycin and clindamycin content of their new method with protein binding constants. Investigated detect potential buffer medium acidity, of separation buffer species, additives, and other conditions of electrophoretic separation and detection results. Under optimized conditions, the three drugs within five minutes to reach the baseline separation, peak area and sample concentration of azithromycin 0.025-2.50μg/mL between roxithromycin 0.50-100μg/mL between and g The clindamycin 0.10-100μg/mL between was a good linear relationship. Concentration 1.00μg/mL mixed samples 6 parallel determinations, the RSD of peak height and migration time between 0.53-1.8% and 0.53-0.57% respectively. Determination of the method for the determination of the three drugs in the pharmaceutical content, and the recovery in 94.6% 1 sup> 04.6% between. And measured three drugs and protein binding constant for the Azithromycin 3.55 × 103 L / mol respectively, the roxithromycin 1.44 × 104 L / mol, clindamycin 1.67 × 104 L / mol. Chapter capillary electrophoresis electroluminescent chemiluminescence determination of ephedrine in ephedra, pseudoephedrine and methyl ephedrine PB-Eu chemical modified electrode as the working electrode, the ionic liquid as a split additive, for the first time to establish capillary electrophoresis electrochemiluminescence The luminescence method for simultaneous separation and detection of a new method of ephedrine, pseudoephedrine and methyl ephedrine. Investigated detect potential buffer medium acidity, of separation buffer species, additives, and other conditions of electrophoretic separation and detection results. Under optimized conditions, the three drugs can be reached within eight minutes baseline separation of its peak area and sample concentration between 0.025 1 sup> 0μg/mL methyl ephedrine, ephedrine 0.025 2 sup> and pseudoephedrine between 5μg/mL linear relationship was good two paragraphs 0.05 1 sup> 0μg/mL between. Of the mixed concentration 1.00μg/mL samples 6 parallel determinations of the peak area and migration time RSD were the 3.95% sup> 4.30% and 0.14% sup> 0.94% between. Determination of the method for the determination of the three substances content of Pharmacy and Chinese Medicine, the recovery of 104.3% 1 sup> 11.2%.
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