Preparation And Recognition Properties Of Cinchonine Bifunctional Monomer Imprinted Materials

Cinchonine and cinchonidine are epimers of each other,and they have different performance in biological activity,pharmacological action and application.At present,cinchonine is used to prevent and control malaria and treat fever,but also because it is used as a catalyst for chiral asymmetric reaction,the reaction conditions are mild and friendly to the environment,so it is more popular.In addition,it can promote the apoptosis process of tumor cells and is expected to be applied in the treatment of cancer in the future.Therefore,it is of great significance to obtain high purity sinkoning in practical application.In this project,two functional monomers,methacrylic acid（MAA）and Allyl-β-cyclodextrin（Allyl-β-CD）,were used to prepare three kinds of surface molecularly imprinted materials.The cyclodextrin-type molecularly imprinted material（MIP-P（Allyl-β-CD）/PSA）,methacrylic acid type molecularly imprinted material（MIP-PMAA/PSA）and double haplotype molecularly imprinted material（MIP-PMAA-（Allyl-β-CD）/PSA）were prepared.The recognition and separation properties of surface molecularly imprinted materials were studied.The results provided theoretical reference for separation of sinkoning.（1）In DMF solvent,ammonium persulfate was used as initiator to initiate the polymerization of polystyrene primary amine resin microspheres with Allyl-β-cyclodextrin to prepare cyclodextrin-type grafted particles（P（Allyl-β-CD）/PSA）.Through a series of experiments,the optimal conditions were as follows: DMF as solvent,0.2g PSA as base,adding 0.35 g functional monomer Allyl-β-CD and 0.4g initiator APS,and reacting at 65℃for 8h,the maximum graft degree of P（Allyl-β-CD）/PSA was 175.56mg/g.A cross-linking agent was added to the grafted polymer with saturated adsorption of cinchonine,and MIP-P（Allyl-β-CD）/PSA was prepared under appropriate conditions.Good identification and separation performance,with a selectivity coefficient of 3.02,can be used for solid phase extraction,and finally achieve the separation of cinchonine and cinchonidine.By examining the elution performance of MIP-P（Allyl-β-CD）/PSA,it was found that the desorption rate within 40 bed volumes was 99.6%,and it had good reusability.（2）In the mixed solution（V ethanol: V water = 1:1）,ammonium persulfate was used as initiator to initiate the polymerization of polystyrene primary amine resin microspheres with methacrylic acid to prepare methacrylic acid type graft particles（PMAA/PSA）.Through a series of experiments,the optimal conditions were as follows: using mixed solution（V ethanol: V water = 1:1）as solvent,0.2g PSA as base,adding 0.6 m L functional monomer MAA and 0.2g initiator APS,and reacting at 60℃ for 8h,the maximum grafting degree of PMAA/PSA prepared was 191.9mg/g.MIP-PMAA/PSA was prepared under appropriate conditions by adding crosslinking agent into the saturated adsorbed graft polymer of cinchonine.The material can separate cinchonine from the mixed solution of cinchonine and cinchonidine,and has good selectivity and separation performance.The selectivity coefficient is 6.26,which can be used for solid phase extraction.Finally,the separation of cinchonine and sinconidine was achieved.By studying the elution performance of MIP-PMAA/PSA,the desorption rate of MIP-PMAA/PSA in 40 bed volume is 99.7%,which has good repeatability.（3）In water,ammonium persulfate is used as an initiator to initiate the polymerization of polystyrene primary amine resin microspheres and methacrylic acid to prepare double monomer graft particles（PMAA-（Allyl-β-CD）/PSA）).Through a series of experiments,the optimal conditions are as follows: the maximum grafting degree of PMAA-（Allyl-β-Cd）/PSA was 209.09mg/g when 0.2g PSA was added into 0.1g Allyl-β-CD,3m L MAA and0.1g APS at 60℃ for 8h.A cross-linking agent was added to the grafted polymer with saturated adsorption of cinchonine,and MIP-PMAA-（Allyl-β-CD）/PSA was prepared under appropriate conditions.It is separated from the solution,has good identification and separation performance,and has a selectivity coefficient of 6.78,which can be used for solid phase extraction for the separation of cinchonine and cinchonidine.By examining the elution performance of MIP-PMAA-（Allyl-β-CD）/PSA,the desorption rate within 40 bed volumes was 95.8%,which has good reusability.