| Abstract: The present thesis consisted of two parts: review and research report. In the review we had reviewed the application of CL detection method and its relayive technology for the minum poison analysis, there are CL method for hydroxybenzene analysis, pesticide analysis, polycyclic aromatic hydrocarbons (PAHs) analysis, toxic gas detection, toxic metal ion analysis, toxic inorganic ion detection and harmful drug analysis, etc.The research report contains three subunits:(1) Ultrasonic digest and nonsegmented continuous droplet flow injection chemiluminescence method for the organophosphorus pesticides analysisBased on the Molybdovanadophosphrate (P-Mo-V) Heteropoly Acid oxidate alkaline luminol produced chemiluminescences. The organophosphorus pesticides were quantitative converted to orthophosphate by ultrasonic couples with oxidant. Then the orthophosphate with molybdate and vanadate to form the vanadomolybdophosphoric (V-Mo-P) Heteropoly Acid. Then the drop flow injection system was used to detect the chemiluminescence's signal. In the present method orthophosphate calibration graph was used for organophosphorus pesticides measurements in the samples. Under the optimal conditions, the CL intensity was linear to the orthophosphate concentration in the range of 1.0×10-8～2.5×10-6 mol/L (r=0.9988, n=7), the detection limit is 3×10-9 mol/L. The relative standard deviation was 3.4% at 1.0×10-7 mol/L (n=11). This method has been successfully applied to the determination of trace dimethoate, dichlorvos, Trichlorfon (Dipterex) residues in vegetables and fruits. The results are good agreement with the reference Spectrophotometry (the Re is less than±4 %). the present method realized rapid (300/h), sensitive, simple detection.(2) Flow injection chemiluminescence method for dexamethasone acetate analysis and reaction mechanism studyA flow-injection chemiluminescence (CL) method coupled with solvent extraction for the determination of dexamethasone acetate (DA) in ointment is presented in this paper. It is based on the enhancing effect of the studied drug on CL emission of luminol-K3Fe(CN)6 systems. This method has the advantages of simple sample treatment, cheap instrumentation and rapid detection. Under the optimum conditions, relative CL intensities are proportional to DA concentrations in the 0.044～4.4μg/mL range. The limit of detection is 0.01μg/mL (3σ) for DA. The method is applied to DA content in commercial DA ointment pharmaceutical and to human skin DA absorption analysis. Experiments are performed to evaluate the nature of DA enhanced luminol-K3Fe(CN)6 chemiluminescence reaction, based on the experimental results we suggest that in this CL system, DA was oxidized by K3Fe(CN)6 to form a medium product (DAox), then DAox oxidize luminol with a faster kinetic step than K3Fe(CN)6 directly oxidize luminol to a active form, as this enhances the luminol-K3Fe(CN)6 chemiluminescence reaction speed. Finally intensify the CL signal.(3) Heterogeneous drop flow injection chemiluminescence studyThe continuous drop flow injection system was used to detection the CL signal of organic extraction solvent directily reacted with the CL reagent in polarity aqueous. Realized the heterogeneous reaction. The sensitive I2-1uminol CL system was chosed as the study model. The experimental results showed that the method realized the reaction of reagents in heterogeneous and has the analytical capability. |
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