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Study On Spectral Properties And Chromatographic Behavior Of Some Drugs And Environmental Pollutants

Posted on:2015-01-08Degree:MasterType:Thesis
Country:ChinaCandidate:B BaiFull Text:PDF
GTID:2251330428463512Subject:Drug Analysis
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Supramolecular chemistry with cucurbituril subject has beendeveloping rapidly in recent years, it has become one of the mostactive research field in supramolecular chemistry, many nonfluorescent or weakly fluorescent species by fluorescence analysismethod of traditional cannot realize the fluorescence measurement,so the measurement becomes in pharmacokinetic monitoring andtrace pollutants in the environment is very difficult. In recent years,new fluorescent probe system cucurbituril-the establishment of ISOquinoline drugs make many non fluorescent drug established theanalysis method of high sensitivity. The purpose of this paper is to usethis new fluorescent probe system, using fluorescence spectroscopy,nuclear magnetic resonance spectroscopy, density functional theoryand other means of interaction from two aspects of experimental and theoretical study of certain drugs and environmental pollutants andcucurbituril subject object between, established the mechanism ofthis probe system and the target analyte a new fluorescence probemethod, the non fluorescent drug and no fluorescence ofenvironmental pollutants. In addition, this paper also uses a self-madenew type chiral stationary successful resolution of19chiralcompounds.1、summarizes the cucurbituril synthesis, structure and features inthe molecular switch, molecular recognition, the advances in thestudy on drug analysis, advances in High Performance LiquidChromatography Chiral compounds is introduced in this paper, themain research contents of this thesis.2、 The no fluorescent drug clenbuterol of cucurbituril [7]–palmatine(PAL) fluorescence quenching complexes by fluorescencespectrophotometry. ΔF has better linear relationship betweenchanges in emission signal in the concentration of0.011-4.2μg mL–1concentration range of drug clenbuterol and fluorescence values,0.9997is the coefficient of correlation, the minimum detection limitwas0.004μg mL–1. Quantitative analysis of clenbuterol residues ofthis method has been successfully applied in pork tissues, therecovery rate is96.05%-97.21%. Another experiment by fluorescence titration method,1H NMR spectrum and molecular modelingcalculations, the clenbuterol and PAL competition reaction andsupramolecular effects on Cucurbit [7] uril cavity mechanis.3、 Hexadecyl trimethyl ammonium bromide(CTAB) has nofluorescence in aqueous solution, and therefore can not be used todetermine the content of direct fluorescence method. In the acidmedium and under the condition of room temperature, PAL cangenerate stable and cucurbituril [7] inclusion and fluorescenceinclusion significantly enhanced. With the addition of CTAB,cucurbituril [7]-PAL fluorescence intensity of complexes weakengradually. Significant quenching of fluorescence intensity of thesupramolecular complexes based, a method for the determination ofaqueous solution of CTAB with high sensitivity and high selectivityfluorescence analysis. In0.070-18μg mL1concentration range ofCTAB concentration and cucurbituril [7]-PAL fluorescence quenchingcomplex values showed a good linear relationship between ΔF, thelowest detection limit was0.023μg mL1. The main object ofexperimental determination of the apparent binding constants, andthe calculation of1H NMR spectrum and molecular model byfluorimetry, studied CTAB and PAL competition reaction andsupramolecular effects on Cucurbit [7] uril cavity mechani. 4、Through the use of D-phenylglycine self-made silica gel chiralstationary phase, by HPLC, using90:10n-hexane-isopropanol asmobile normal phase chromatographic conditions, and80:20acetonitrile water (containing0.1%three triethylamine acetic acidpH=4.2buffer solution as mobile phase inverting) thechromatographic conditions,19kinds of chiral drugs were separated.The experimental results show that: the chromatographic stationaryphase on the contrary chromatography conditions can complementeach other very well. For the determination of chiral drugs, not to theresolution of chiral drugs can get better resolution in reversed phasechromatographic conditions in normal phase chromatographicconditions, while in the chiral drugs cannot be split reversed-phasechromatography conditions can obtain chiral resolution well innormal phase chromatographic conditions. Has been good for mostresolution of chiral drugs, is a good chiral separation ability to chiralstationary phase.
Keywords/Search Tags:cucurbit [7] uril, CTAB, clenbuterol, D-phenylglycine, fluorescence titration, fluorescence probe, HPLC, chiral separation
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