Open-tubular Capillary Electrochromatography For The Analysis Of Acid Drug

Open-tubular capillary electrochromatography (OTCEC) is an emergingmicrocolumn electroseparation technique which combines the high selectivity ofHPLC and the high efficiecy of HPCE. The stationary phase is coated or eroded onthe wall of capillary, whereas the mobile phase moves through the column propelledby electroosmosis. It has recently received considerable attention and been applied infood safety detection, medicine anslysis and other areas.Phenoxy acid herbicide is a kind of systemic herbicides that is widely used incorn, rice, wheat and other agricultural production. Various reliable and sensitivedetection methods have been investigated due to its potential carcinogenicity andaberration inducing effects. Domoic acid (DA), the main component of the Marinebiotoxin Amnesic Shellfish Poisoning (ASP), has strong neurotoxicity which cancause persistent short-term memory impairment. After consumption of contaminatedfish or shellfish, serious illness will occur. Canada was the first country to set a limitfor DA with the regulatory level of20μg/g total tissues. So, it is very significant inpractice and theory to study the OTCEC-UV technique and its application inphenoxy acid herbicides and amnesic shellfish poisoning analysis for extending therange of the application of CEC and promoting the development of the subject.In chapter1, a brief review of OTCEC was generally introduced. Thepreparation of OTCEC was described in detail. Furthermore, the on-lineconcentration technique of CEC was reviewed. And then, on this basis, the aim andsignificance of this thesis were briefly presented.In chapter2, a new system of OTCEC-UV detection to the analysis for DA wasdeveloped by our group. The buffer type, buffer pH, concentration of buffer,separation voltage, injection time, injection voltage and other important factors weresystemically investigated and optimized. Under the optimal conditions, DA can bedirectly detected in short time. The detection limit was1.0μg/g total tissues and themean recoveries ranged from80.5％～83.1％. This detection method had features ofsimple steps, easy control, short analysis time and low sample consumption and soon. Therefore, it had great significance for the control and detection of domoic acid in shellfish.In chapter3, the triamine-bonded open-tubular capillary column prepared byour group had characteristics of capillary electrophoresis effect and ion-exchange.Combining it with the Field Amplified Sample Stacking (FASS) technique, a newmethod to analyse phenoxy acid herbicides was established. The effects ofchromatographic separation conditions were systemically investigated and optimized.Under the optimal conditions,2,4-D,2,3-CPPA,2-2CPPA and2-PPA wereefficiently separated with satisfactory results, and their detection limits were5.0×10-8mol/L,5.0×10-8mol/L,8.0×10-8mol/L and8.0×10-8mol/L. The methodwas applied to the determination of four phenoxy acid herbicides in agriculturalwastewater with good results, and the average recovery was between84.0%~92.3%.Compared with pressurized capillary electrochromatography, this method had lowersample consumption and lower cost, and offered a new way for analysis of phenoxyacid herbicides.