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Study On Pharmaceutical Analysis By Using Capillary Electrophoresis With Electrochemiluminescence

Posted on:2008-12-04Degree:MasterType:Thesis
Country:ChinaCandidate:Y H KangFull Text:PDF
GTID:2144360215483309Subject:Analytical Chemistry
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Capillary electrophoresis (CE), is also known as high performance capillary electrophoresis (HPCE). Comparing with the traditional separation methods, CE has become an important analytical tool because of its powerful separation capacity, high efficiency, short analytical time, and minimum consumption of sample and reagents. In addition, it also has an economic, clean, easy automation, and multi-purpose small environmental advantages. Electrochemiluminescence (ECL) known as electrogenerated chemiluminescence, it is a product that combines the electrochemical methods and chemiluminescence method. ECL detection with Ru(bpy)32+ is a viable alternative for CE detection. ECL has the advantages of simplicity, inexpensive instrumentation, low background noise, high sensitivity, good selectivity, and wide dynamic linear range. Their high sensitivity, simplicity and wide linear range make electrochemiluminescence as a powerful detector of capillary electrophoresis. So, the marriage of CE to ECL (CE-ECL) offers the merits with enhancing sensitivity, improving selectivity, and reducing cost. It is become a sensitive and efficient analytical technique. CE-ECL detection is widely used in various fields, such as in pharmaceutical analysis, bio-analysis, food analysis, the separation and analysis of other samples.This thesis is concentrated on the application of CE-ECL detection using Ru(bpy)32+ for the analysis of pharmaceuticals. Its main contents were introduced as followings:1. Erythromycin, an important macrolide antibiotic, was detected by CE-ECL using Ru(bpy)32+ regent . This CE-ECL detection method has high sensitivity, good selectivity and reproducibility for erythromycin analysis. Under optimized conditions, the ECL intensity was linear with the erythromycin concentration in the range of 1.0×10-9~1.0×10-5 g/mL. The detection limits (S/N = 3) for erythromycin was 3.5×10-10 g/mL. When the method was applied to determine erythromycin in rat plasma, the recoveries were between 91.4% and 100%.2. CE-ECL detection of josamycin in rat plasma based on Ru(bpy)32+ was described. After CE separation using a 75μm i.d. uncoated capillary column and 15 mmol·L?1 running buffer solution at 12 kV of separation potential, the analyte was detected at the surface of platinum disk working electrode. Parameters that affect separation and detection were optimized. Calibration curve was linear over the range from 1.0×10-8 g/mL to 5.0×10-6 g/mL with a detection limit of (S/N = 3) 3.1×10-9 g/mL. The method can be successfully applied for the determination of josamycin in rat plasma. The recoveries were between 90.9 and 95.5%.3. A method of CE with ECL detection has been applied to the determination of haloperidol. Under optimal conditions, the ECL intensity was linear with the haloperidol concentration in the range of 1.0×10-8~1.0×10-5 g/mL. The detection limits (S/N=3) for haloperidol was 3.5×10-9 g/ mL, and the RSD was 5.0% for 3.0μg/mL haloperidol (n = 9). When the method was applied to determine haloperidol, the recoveries were between 90.8% and 95.7%.4. Simultaneous determination of erythromycin (Ery) and haloperidol (Hal) in human urine by CE with ECL detection. Under optimized conditions, such as detection potential at 1.25 V, electrokinetic injection at 10 kV for 6 s, separation voltage at 10 kV, 15 mmol/L separation buffer with pH 6.5, 5 mmol/L Ru(bpy)32+ and 50 mmol/L phosphate buffer with pH 8.0 in the ECL cell, the linear range were 0.005~0.2μg/mL for Ery and 0.15~6.0μg/mL for Hal. The detection limits (S/N = 3) for Ery and Hal were 0.002 and 0.06μg/mL, respectively.
Keywords/Search Tags:Capillary electrophoresis, Electrochemiluminescence, Pharmaceutical analysis, Tris(2,2′-bipyridyl)ruthenium(II)
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