| High Performance Liquid Chromatography is one of the most important methods for modern separation and analysis of compounds.The pursuit of rapid liquid separation technology has promoted the development of new chromatographic techniques.In recent years,with the extensive use of small particle size packing materials and the rise of Ultra-High Performance Liquid Chromatography,in order to reduce the increasing cost of instruments,the new core-shell chromatographic packing material has been developed.This new material is prepared by melting porous silicon shell onto the surface of solid silicon nucleus,which brings high speed,high efficiency,high sensitivity and low colμmn pressure,and ensures the same resolution as Ultra-High Performance Liquid Chromatography on common liquid chromatograph.This paper studies a new type of chromatographic packing material with core-shell chromatographic silica gel as matrix,the preparation of the stationary phase bonded with organic/inorganic pentafluorophenol(PFP),the characterization of its physical and chemical performance and the test of its chromatographic performance in the separation of different compounds.The study leads to the following conclusions:1.The organic/inorganic hybrid polymer,prepared with TEOS and triethylsilane,and reacts with Ultra-pure core-shell silica base and produces an organic/inorganic hybrid layer on the surface,with higher pH tolerance and wider pH range(1.5-12).On this basis,bonded PFP groups on the surface brings special selectivity of stationary phase and higher retention for polar compounds.Use various characterization techniques to characterize the prepared stationary phase and the resul ts showed its regul ar surface,narrow particle distribution and good thermostability.Compared with porous chromatographic packing materials,this stationary phase has higher chromatographic performance,including higher resolution,higher analysis speed and lower column pressure.Through pH tolerance test,this stationary phase shows good stability at pH 12 and good tolerance under alkaline condition.2.The performance of the prepared stationary phase in the separation of different compounds:(1)Taxol and related substances.Through application experiments of taxol,this stationary phase shows better performance than that of porous PFP stationary phase.It has greatly shortened the analysis time and developed new chromatographic methods for taxol and related substances.(2)10 common Anthocyanins.Compared with porous C18 stationary phase and phenyl stationary phase,this bonded stationary phase provides better resolution,better selectivity and higher analysis speed.It has developed a new HPLC method for 10 Anthocyanins.3.An organic/inorganic hybrid C18 core-shell stationary phase prepared,using Ultra-pure bare core-shell silica as matrix.After being characterized with various characterization techniques,it was packed to column and used in the separation of Ginsenoside.The resul ts indicate that it has accurate detection of Ginsenoside Rgl,Rb1 and Re,with high analysis speed,high accuracy and high sensitivity.The new HPLC method for ginsenoside has also been developed. |
