Preparation Of Restrict Access Material And Its Application In Medicine Analysis

In this paper,the reversed phase restrict access material and magnetic reversed phase restrict access material were prepared via atom transfer radical polymerization(ATRP),respectively.The adsorption property to small molecules and the exclusion ability to proteins were investigated in detail.The reversed phase restrict access material was used as the sorbent to separate and enrich the oxytetracycline in saled milk.The magnetic reversed phase restrict access material were used as the solid phase matrix.It was used to separate and enrich the sulfonamides in bovine serum and milk samples.The chloramphenicol restricted access media-molecularly imprinted polymers(CAP-RAM-MIPs)were prepared by precipitation polymerization.The result has shown that CAP-RAM-MIPs not only have the selectivity for the template but also have the ability of exclusion for bovine serum albumin(BSA).The adsorption characters were studied by adsorption isothermal,kinetic,thermodynamics and selectivity in detail.The solid phase extraction coupled with high performance liquid chromatography and ultraviolet(HPLC/UV)were applied to determine chloramphenicol in bovine serum sample.The paper consists of the following parts:1.In this work,A reversed phase restrict access material was prepared via two steps of atom transfer radical polymerization(ATRP).The octadecyl methacrylate(C18)and glycidylmethacrylate(GMA)were grafted on inner and outer surface of modified silica.After hydrolysis,gotten a hydrophilic reversed phase restrict access material with rich glycol group.It was characterized by fourier transform infrared(FT-IR)spectrum,element analysis and thermogravimetric(TGA)analysis.They all indicated that C18 and GMA were grafted successfully.The static adsorption experiment was employed for evaluating the binding capacity and the maximum adsorption amount of sulfadimethoxine and oxytetracycline were 18.02 mg/g and 4.80 mg/g,respectively.The exclusion ability to proteins like bovine serum albumin(BSA)was up to 90%.The novel reversed phase restrict access material was used to separate and enrich the oxytetracycline in milk.The high performance liquid chromatography(HPLC)was used to detect it and the average recovery was 89.19%,the relative standard deviation(RSD)was 3.03%.2.The Fe2O3 has been synthesized by the method of solid state grinding at room temperature.The magnetic reversed phase restrict access material was prepared via atom transfer radical polymerization(ATRP)on the surface of Fe2O3/SiO2.The octadecyl methacrylate(C18)and glycidylmethacrylate(GMA)were grafted on inner and outer surface of Fe2O3/SiO2,allowing brominated Fe2O3/SiO2 and CuBr/2,2-pyridine to serve as macro-initiator and catalyst system.After hydrolysis,a magnetic material with rich glycol group was prepared.It was characterized by x-ray powder diffraction(XRD),element analysis and scanning electron microscopy(SEM).By means of methyleneblue adsorption methods to calculate the surface area of magnetic reversed phase restrict access material and the vaule was 5.235 m2/g.The properties of material for the exclusion of proteins like bovine serum albumin(BSA)were evaluated using solid-phase extraction(SPE)and its exclusion value up to 90%,significantly surpass the unopening material.The maximum adsorption amount of sulfadimethoxine,sulfisoxazole,trimethoprim and sulfamerazine were 2.24 mg/g,2.76 mg/g,1.51 mg/g and 1.34 mg/g,respectively.The magnetic reversed phase restrict access material were used for separation and enrichment of sulfonamides in bovine serum and milk samples,detected by HPLC and got good results.3.The chloramphenicol restricted access media-molecularly imprinted polymers(CAP-RAM-MIPs)were prepared by precipitation polymerization.The chloramphenicol,acetonitrile and glycidilmethacrylate(GMA.)were chosen as template molecule,solvent,hydrophilic functional monomer,respectively.It was characterized by fourier transform infrared(FT-IR)spectrum,scanning electron microscopy(SEM)and thermogravimetric(TGA)analysis.The adsorption characters were studied by adsorption isothermal,kinetic,thermodynamics and selectivity in detail.The maximum adsorption amount of CAP-RAM-MIPs was 278.3 mg/g,which is superior to other reports.Compared with its analogues like thiamphenicol and florfenicol,it possesses a good selectivity to chloramphenicol.The equilibrium adsorption datas were fitted well to both Langmuir and Freundlich isotherms.The pseudo-first-order and pseudo-second-order reaction kinetic fitting curves of CAP-RAM-MIPs indicated that the adsorption process was second-order kinetics.The polymers were used as solid phase extraction packing to separation and enrichment of chloramphenicol from bovine serum sample.The high performance liquid chromatography and ultraviolet(HPLC/UV)was successfully applied to determine it.The average addition standard recoveries were among 105.22%?120.11%,the relative standard deviations(RSD)were 0.0065%?0.039%.