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Study On Analysis Of Pharmaceutical And Pesticide Residue Using Chemiluminescence

Posted on:2008-07-29Degree:MasterType:Thesis
Country:ChinaCandidate:N XiaoFull Text:PDF
GTID:2143360215465038Subject:Biochemistry and Molecular Biology
Abstract/Summary:PDF Full Text Request
Chemiluminescence (CL) analysis, based on the emission during some chemical reactions, is a technique for the determination of trace analyte. Due to its high sensitivity, wide linear range and easy implementation, chemiluminescence analysis has been widely applied in pharmaceutical analysis, food safety, environmental science and life science etc. In this thesis three different CL systems, luminol-KIO4 CL system, luminol-KMnO4 CL system, alkaline luminol CL system, were introduced to detect some pharmaceuticals and the residue of pesticides using a flow injection chemiluminescence (FI-CL) method. The main content is as following:1. A simple chemiluminescence method for the determination of hydrochloride adrenaline with flow injection chemiluminescence (FI-CL) technique was proposed, which was based on hydrochloride adrenaline enhancing the chemiluminescence from potassium periodate and luminol in alkaline medimum. The linear range of the calibration curve was 1.0×10-8~3.0×10-6g/mL, and the detection limit was 1.5×10-9g/mL. The relative standard deviation was 1.3%(n=11, c=5×10-7g/mL,). The method has been applied to the determination of hydrochloride adrenaline in pharmaceutical samples.2. It was found that the chemiluminescence arising from the reaction of luminol with potassium permanganate in alkaline solution could be strongly enhanced by metaraminol bitartrate. Based on these observations, a new flow injection chemiluminescence (FI-CL) method for the determination of metaraminol bitartrate was proposed. The linear relationship between the intensity of chemiluminescence and the concentration of metaraminol bitartrate was in the range of 1.0×10-8~1.0×10-5g/mL with a detection limit of 3.7×10-9g/mL and the relative standard deviation was 2.5%(n=11, c=1.0×10-7g/mL). The method was successfully applied to the determination of metaraminol bitartrate in its pharmaceutical formulations. Moreover the reaction mechanism of the chemiluminescence system has been discussed based up on the fluorescent spectra, UV-visible spectra and some other experiments.3. A flow-injection chemiluninenscence (FI-CL) method was set up for determination of organophosphate pesticides in vegetables. The degradation of organophosphate pesticides can be achieved by photo-catalysis in K2S2O8 solution. The inorganic phosphorus (the products of degradation of organophosphate pesticides) could form vanadomolybdophosphoric heteropoly acid with the addition of vanadate and molybdaenate in sulfuric acid medium, which could oxidize luminol to produce CL emission. The CL emission intensity was linearly correlated with the phosphorus concentration in the range 1.0×10-9~3.0×10-6g/mL with a detection limit of 1.0×10-10g/mL. The relative standard deviation (n=11) was 2.1%for 2.0×10-7g/mL phosphorus. The recoveries ranged from 89.5%to 114%by adding 3 different organophosphate pesticides with amount of 1.00mg, 2.00mg pesticide per kilogram vegetable respectively. The method has been applied satisfactorily to the determination of organophosphate pesticides on mini chemiluminescence instrument.
Keywords/Search Tags:Chemiluminescence analysis, Flow-injection analysis, Hydrochloride adrenaline, Metaraminol bitartrate, Organophosphate pesticides
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