氢化松香酯键合硅胶制备柱的研制及性能研究OA北大核心CSTPCD

Hydrogenated rosin glycol acrylate(EGHRA)was bonded to the surface of thioglycolated silica gel(SH@SiO2)by click chemical reaction to prepare a novel hydrogenated rosin acrylate ethylene glycol ester bonded silica gel(EGHRA@SiO2)stationary phase.The synthesized stationary phase was characterized by elemental analysis,infrared spectroscopy,thermogravimetric analysis,N2 adsorption-desorption experiments,and particle size distribution tests.The results showed that the EGHRA@SiO2 stationary phase had an increased C content of 10.72 percentage points compared to SiO2,a specific surface area of 270.06 m2/g,an average pore diameter of 6.16 nm,and an average particle size of 10 μm.A 250 mm×30 mm preparation column was filled by homogenization method,and a series of chromatographic evaluations were performed,demonstrating good flowability typical reversed-phase chromatographic characteristic as well as excellent stability and reproducibility of the EGHRA@SiO2 preparation column.Tanaka tests showed that the spatial selectivity of EGHRA@SiO2 column was superior to that of C18 column owing to the phenanthrene-like skeleton of the bonding monomer.Under reversed-phase chromatographic mode,EGHRA@SiO2 preparation column exhibited ideal separation performance for the crude extracts of Taxus bark.Using the screened acetonitrile-water(volume ratio of 47∶53)mobile phase at a flow rate of 15 mL/min,the purity of paclitaxel(PTX),10-deacetylbaccatin Ⅲ(10-DAT),7-xylosyl-10-deacetylbaccatin Ⅲ(7-xyl-10-DAT)and cephalomannine(CEP)in the crude extract were increased by 91.52,83.24,62.99 and 55.85 percentage points after a single purification step of 1.0 mL injection sample,respectively.