Preparation,Characterization And Application Of Polar Group Embedded C30 Chromatography Packing

High-performance liquid chromatography(HPLC)is widely used in various research domain because of its faster analysis speed,simple conditions and universal applicability.It has become the most practical analytical technology.The stationary phase technology that is core of HPLC is constantly evolving.In the history of chromatography,C18 was the most commonly used stationary phase that can separate some substances.But C18 had the poor peak shape when separating alkaline substances or easily dissociated substances.This problem was solved by embedding the polar group in the C18 stationary phase.But its shape selectivity was poor.It was difficult to achieve the ideal separation when separating structural similar substances.In the above background,the full porous silica gel was used as the matrix in this study.The polar urea-propyl C30 stationary phase(TPU-C30)was firstly prepared by embedding the polar group of urethane into C30 in two steps.Its physical properties and chemical properties were analyzed.And we also explored its column performance and column application.The conclusions were obtained:1.A novel polar urea-propyl-C30 stationary phase was prepared by using3-ureidopropyltrimethoxysilane as a coupling agent.The physical characteristics of TPU-C30 stationary phase were analyzed by SEM,FT-IR,elemental analysis,specific surface and pore size analyzer,thermogravimetric analyzer and the like.The results indicated that TPU-C30 stationary phase had been successfully synthesized in this study.The fixed phase exhibited some advantages,including uniform morphology,uniform particle size,suitable surface area and feasible pore size(specific surface area was 114.4 m~2/g,pore diameter was 7.4 nm).The carbon content of TPU-C30 was 13.86%.The thermal stability of TPU-C30 stationary phase was also good.And it belonged to the mesoporous material.2.The stability and chromatographic performance of the TPU-C30 stationary phase was investigated.The test results of TPU-C30 stationary phase were compared with the traditional C18 stationary phase and C30 stationary phase:(1)Test the performance of the column with toluene as the sample solute.The results showed that the TPU-C30 stationary phase had good stability and low detection limit.(2)The polarity and hydrophobicity of the TPU-C30 stationary phase were also investigated.The results showed that the stationary phase was polar.(3)The separating properties of polar and non-polar substances were investigated with TPU-C30 stationary phase.The experimental results showed that the TPU-C30 stationary phase had different sample selectivity from the C18 stationary phase and C30 stationary phase.(4)The shape selectivity of TPU-C30 stationary phase was investigated too.The experimental results showed that the TPU-C30 stationary phase had better shape-selective properties than C18 stationary phase and C30 stationary phase.(5)The amitriptyline was analyzed by TPU-C30 stationary phase.The experimental results showed that the TPU-C30 stationary phase had a good peak shape when separating alkaline substances.3.Sample types that was suitable for TPU-C30 column were investigated.And we also developed the new sample analysis methods.(1)The application of TPU-C30column in the common four nucleosides was explored.The experimental results showed that the TPU-C30 column provided a new choice for the analysis of nucleosides.(2)The application of TPU-C30 column in allantoin was explored.The experimental results showed that the chromatogram could further improve the purity of the allantoin.(3)The application of TPU-C30 column in sorbic acid,benzoic acid and dimethyl fumarate was explored.The experimental results showed that the column achieved good separation effect on these substances.The TPU-C30 stationary phase can be applied in various fields.