Study On The Preparation Of MAA,TMPTA Polymer And Phenyl Hybrid HPLC Monolithic Columns For The Separation Of Small Molecular Drugs

In this paper,two new polymers and an organic hybrid high performance liquid chromatography(HPLC)monolithic columns were prepared.The column was used as the chromatographic stationary phase.It was expected to establish a new method of efficient,fast,simple and green for separating small molecular drugs in biological samples by HPLC.The main research work is as follows:1)Using the classical free radical polymerization method,methacrylate(MAA)as monomer and dimethacrylate as crosslinking agents were used to prepare organic polymer monolithic column.The factors influencing the preparation of MAA organic polymer monoliths were studied systematically.The structure was characterized by scanning electron microscopy(SEM)and infrared spectroscopy(FT-IR),and the chromatographic properties of benzene,naphthalene and phenanthrene were evaluated as hydrophobic modes.And the optimized preparing poly(methacrylic acid-1,6 hexanediol dimethacrylate)(MAA-HDDMA)was used as an HPLC stationary phase to separate two groups of basic small molecular drugs.Although the mechanical properties,permeability and stability of the monolith prepared by the optimized conditions are good,and the selectivity of the small molecule drugs is different,the separation ability and the column efficiency are not ideal.2)Poly trimethylolpropane triacrylate(TMPTA)monolithic column was prepared by optimizing the ratio of reactants and polymerization time by ultra-high cross-linking polymerization technique with good permeability,mechanical strength and good column efficiency.And as a HPLC stationary phase combined with a new method of pure water micellar liquid chromatography to separate the four groups of small molecular drugs for green and rapid separation.At the same time,it was applied to analysis the serum of three kinds of anti-angina drugs and two kinds of cold medicine components.Although the separation effect did not achieve the desired results,it can not actually determine the serum of these small molecule drugs.But the analysis results showed that the monolithic column have the features of water resistance and micellar green analysis,which can provide a reference to small molecules in serum for the green,efficient,rapid analysis and clinical blood concentration monitoring.3)Using sol-gel method,ethyltetraethoxysilane(TEOS)as the cross-linking agent,phenyl triethoxysilane(PTES)as the organic functional monomer,by changing the polycondensation conditions of two-step acid catalyzed to hydrolysis and alkali-catalyzed,high performance liquid chromatography phenyl hybrid monolithic column was prepared.The influence of factors on the performance of the monolithic column was discussed.In this study,although the advantages of poor mechanical strength,high column pressure and poor reproducibility were overcome,and the optimum conditions and techniques for the preparation of monolithic columns were mastered,the chromatographic separation did not achieve the desired effect.