| Molecular luminescence analysis includes chemliluminescence analysis(including bioluminescence analysis), molecular fluorescence analysis and molecularphosphorescence analysis. Because of its high sensitivity, low detection limit and widelinear range, it has been widely applied to the fileds such as the living science, materialscience, clinical medicine, environment control and pharmaceutical analysis and so on.This thesis mainly studies the applications of fluorescence analysis andchemliluminescence analysis in pharmaceutical.The thesis consists of two parts. The first part is a review in which it introduces thepretreatment methods of solid phase extraction, solid phase micro-extraction,supercritical fluid extraction, membrane separation, microwave, and derivatization, andsummarizes the applications of these pretreatment methods in analytical chemistry inrecent years.The second part is the research report which is composed of 3 parts as follows.First is the the sono-oxidation pretreatment method for the fluorescence analysis of folicacid. Second is the FI-CL method for perphenazine analysis and the mechanismpreliminary study. Third is the formaldehyde test paper research.1. The fluorescence of folic acid was weak. It was found that under the ultrasonicirradiation, folic acid could be oxidized to pterin-6-carboxylic acid in neutral medium.The formation of pterin-6-carboxylic acid exhibited a significant enhancement in thefluorescence intensity far beyond that of native FA at 462 nm of emission wavelength.Based on above phenomenon, a pretreatment method of sono-oxidition based folic acidfluorescence detection was proposed. The proposed pretreatment method was timeefficiency. Moreover, this technique avoided chemical oxidants consumption. Under theoptimal conditions, the linear concentration range of application was 1.0×10-8～2.5×10-6g·mL-1 of folic acid; with a relative standard deviation of 2.6％(for a level of 3.0×10-7g·mL-1; n=11) and a detection limit of 3×10-9 g·mL-1. Folic acid contents in commercialformulations were analyzed with presented method. The feasibility of thissono-oxidation fluorescence method was demonstrated by comparing with thereferenced FA detection method. 2. In the NaOH solution, perphenazine could obviously sensitize thechemiluminesence (CL) intensity of the reaction of luminol with potassium ferricyanide,and the sensitized CL intensity was proportional to the concentration of perphenazine.So, a new flow injection CL method has been developed, and the optimum chemicalconditions for the CL reaction were investigated. Under the optimized conditions,perphenazines were determined. The linear range of the working curves was 1.0×10-8-2.0×10-6 mol·L-1; the detection limit was 3×10-9 mol·L-1; the relative standard deviationwas 2.1％(C=3.0×10-7 mol·L-1; n=11). The method was simple, rapid, and sensitive.The analysis results obtained from presented method were compared with thoseobtained from the pharmacopoeia method.3. Formaldehyde is a kind of protoplasmic poison, which could terribly damage thehuman body. The phenomenon of illegally using formaldehyde as the antiseptic in thefood was comparatively serious at present. Consequently, both consumer and thedepartment of the industrial and commercial skill supervise needed a kind of swift,simple and low-priced method to monitor the existence of the formaldehyde. Accordingto the above, we have designed the test paper which can examine the formaldehyde inthe food quickly, simply and conveniently. This test paper responded rapidly andalternatively to formaldehyde, it was able to realize swift, convenient, low-price, in situdetermination. |
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