The Preparation,Characterization And Application Of Solid Structure Chromatographic Packing

As an efficient and fast analytical separation technology,High Performance Liquid Chromatography(HPLC)has been widely used in component analysis,preparation,separation and purity test.It is an indispensable way of analysis and separation in chemistry and biology laboratory.Chromatographic column is a critical part of the chromatographic system,and the development of chromatographic stationary phase is the core of chromatography technology.The most commonly used reversed phase chromatographic stationary phase is the C18 bonded stationary phase on the silica gel substrate.The C18 stationary phase works well for separating non polar and neutral substances,but because of its strong hydrophobic functional group,it does not work well for retaining highly polar samples.As a result,samples with strong polarity often cannot achieve the ideal separation effect with C18 stationary phase.In addition,for samples of highly similar molecular structure,such as isomers,C18 stationary phase often does not produce ideal separations.To overcome the above mentioned shortcomings of the conventional reversed phase stationary phase such as C18 phase,we synthesized and characterized a new stationary phase which is based on a 3-dimensional structure functional group,adamantane,which is bonded to the surface of silica.The physical and chemical properties of this new stationary phase are characterized,and its chromatographic properties in various compounds are investigated.The conclusions are as follows:1.based on the reaction of ultra-pure spherical porous silica media and adamantylethyltrichlorosilane,a solid cage-like adamantane function group is formed on the surface of silica particles.The physical and chemical structure of this stationary phase were characterized by means of FT-1R,BET,particle-size analysis and elemental analysis.From the characterization results,a stationary phase based on a 3-dimensional functional group was successfully synthesized.The surface area is 331.78 m2/g,the average pore size is 8.36 nm,and the carbon loading is 12%,which belongs to mesoporous material.2.The chromatographic performance of the 3-dimensional structure stationary phase for the separation of different kinds of compounds was investigated and compared with the conventional C18 stationary phase:(1)the hydrophobicity of the 3-dimensional structure stationary phase and the SRM870 method are investigated,the experimental results show that the 3-dimensional structure is mainly hydrophobic when separating non polar samples,and the hydrophobicity is weaker than the conventional C18 stationary phase,it shows that the 3-dimensional structure stationary phase is a reverse phase,and there is a difference between the C18 stationary phase;(2)3 isomers(triphenylene,benao(a)anthracene,chrysene)in polycyclic aromatic hydrocarbons(PAHs)were separated and analyzed by 3-dimensional structure stationary phase,the experimental results show that the 3-dimensional structure stationary phase has good separation and high column efficiency,it shows that it has a special stereoselectivity;(3)the chromatographic performance application of the 3-dimensional structure stationary phase on the separation and analysis of metformin hydrochloride and its impurities and 7 kinds of organic acids was investigated,the experimental results show that the separation of metformin and 7 organic acids by the 3-dimensional structure stationary phase is better than that of C18 stationary phase,and the separation effect is better.We believe that this new 3-dimensional structure stationary phase can be widely used in the fields of biomedicine,food safety and environmental testing.