| Open-tubular capillary electrochromatography is a kind of novel separation andanalytical technique. It’s becoming a promising research field due to its highefficiency, rapid separation and small sample comsumption. Electrochemilumi-nescence has been widely studyed because it needn’t light sources and provides highsensitivity as well as simple instrument. Although research on those two aspects isvery hot, the relative report about OTCEC coupled with ECL has been very few tillnow. In this thesis, open-tubular capillary electrochromatography coupled withelectrochemiluminescence detection method was developed and was also applied tothe analysis of micro-antibiotics.The first part of this thesis is the general introduction, including thedevelopment of OTCEC, the principle of ECL and the technique of coupling withother separation methods. Finally, the aim and significance of this thesis were alsobriefly described.In the second part, by applying triamine-bonded capillary column, theapplication of open tubular capillary electrochromatography coupled withelectrochemiluminescence detection in clindamycin antibiotic analysis wasdeveloped for the first time. Experiment parameters such as pH, buffer concentrationof mobile phase and effecet of applied voltage were studied and optimized. Underthe optimal condition, based on interaction and electrostatic repulsion between thestationary phase and analyte, under the optimal condition, lincomycin andclindamycin were separated to baseline in24min. The limit of quantitation was6×10-8mol/L. This method of analysis for clindamycin antibiotic was developedwhich avoiding the restriction of UV detection.In the third part, by applying cyano-bonded capillary column, the application ofopen tubular capillary electrochromatography coupled with electrochemilumine-scence detection in basic clindamycin antibiotic analysis was developed for the firsttime. The separation behavior of the clindamycin antibiotic based on electroosmotic flow provided by carboxyl groups in the inner face of the column and theinteraction between the stationary phase and basic amine of the analytes. Under theoptimal condition, lincomycin and clindamycin were separated to baseline in10min.The limit of quantitation were6×10-8mol/L and7×10-8mol/L respectively. And therecovery was74.63%-93.16%when applying fish sample. A new sensitive and highefficient method of analysis for clindamycin antibiotic was developed.In the fourth part, based on the electroosmotic flow provided by carboxylgroups in the inner face of the column and the interaction between the stationaryphase and analyte, by applying cyano-bonded capillary column, the application ofopen tubular capillary electrochromatography coupled with electrochemilumine-scence detection in fluoroquinolones antibiotic analysis was developed for the firsttime. Under the optimal condition, five fluoroquinolones(Lomefloxacin, Ofloxacin,Enoxacin, Ciprofloxacin and Norfloxacin) were separated to baseline in15min. Thelimit of quantitation was3.0×10-7mol/L. The recovery was81.60%-100.71%whenapplying fish sample. A new method for cyano-bonded capillary column couplingwith OTCEC-ECL was developed.on the basis of experiment above, the applicationof cyano-bonded capillary column in OTCEC-ECL was broadened. |
