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Preparation Of Solid Phase Extraction Column And Its Application In Food Safety Inspection

Posted on:2014-08-09Degree:MasterType:Thesis
Country:ChinaCandidate:B JiaFull Text:PDF
GTID:2251330401470192Subject:Analytical Chemistry
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Solid phase extraction (SPE) is a technique of treating processes。It use adsorptionbetween adsorbent and target compounds in sample to separate the matrix of targets and chaffinterferent,and then elute the target compounds with eluant to reach the purpose of separationand enrichment enrichment in complex samples.The polystyrene (PS)-methacrylic acid/titanium dioxide composite microspheres were prepared by emulsion polymerization withemulsion polymerization,styrene and tetrabutyl titanate as raw material in the system ofwater/ethanol.The structure was characterized by FT-IR,SEM,X-energy spectrum andtransmission electron microscope.Solid phase microextraction columella was made bypolystyrene(PS)-methacrylic acid/titanium dioxide composite microspheres.With thecoupling technique of SPE-HPLC concentrate the target compounds to analyse by HPLC.Thestandard curve of fenfluramine,ephedrine hydrochloride and sibutramine hydrochloride weredrawed and determinated the content of the hydrochloric acid fluorine ramin, ephedrinehydrochloride and sibutramine hydrochloride in the food and health care products. The bestHPLC condition was determined depending on the influence of solid phase extraction columnperformance the eluant type and mobile phase flow rate.The results show that the SPE ofhomemade had a high extraction rate for hydrochloric acid fluorine ramin, ephedrinehydrochloride and SPE-HPLC had high separation efficiency, good selectivity and analysisquickly. The extraction rate of hydrochloric acid fluorine and ephedrine hydrochloride areboth over90%。 In the range from0.1~0.5mg/mL、0.13~0.52mg/mL、0.065~0.52mg/mL,the relationship between the peak area and concentration of hydrochloric acidfluorine ramin, ephedrine hydrochloride and sibutramine hydrochloride were linear.Degree ofprecision of hydrochloric acid fluorine ramin, ephedrine hydrochloride and sibutraminehydrochloride are4.29%,4.90%and3.89%separately and the limit of detection are0.034mg/L,0.101mg/L and0.018mg/L.Standard addition recovery rate of hydrochloric acidfluorine ramin was from94.7%to102.2%.
Keywords/Search Tags:PS-MAA/TiO2Composite Microsphere, Solid phase extraction, HighPerformance Liquid Chromatography, Fenfluramine Hydrochloride, Ephedrine Hydrochloride, Sibutramine Hydrochloride
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