核壳型SiO2@松香基高分子高效液相制备柱的制备及其对喜树碱的分离纯化

doi:10.3969/j.issn.0253-2417.2021.06.009

Abstract

Abstract:

The silanated silica gels was synthesised by modifing the activated spherical silica gels. Methacrylic acid was uesd as functional monomer, glycol maleated rosinate modified acrylic acid and azobisisobutyronitrile were used as crosslinking agent and initiator. They were mixed and evenly coated on the surface of the silanated silica gels, and then the core-shell SiO₂@rosin-based polymer(SiO₂@R) chromatography stationary phase was synthesised by coating-suspension free radical polymerization. The stationary phase was characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, thermogravimetric analysis, specific surface area and microporous adsorption analysis. The results showed that the rosin polymer was successfully bonded on the surface of silica gel, the core-shell SiO₂@R stationary phase was successfully prepared, and the cytotoxicity of stationary phase was lower than that of commercial resin.The high performance liquid preparative chromatographic column(30 mm×250 mm, 10 μm) was prepared by wet packing. And its performance was tested. The results showed that the particle size of the theoretical plate number of the preparative column was 59 992, it had good liquidity and reusability. Methanol-water(volume ratio 95∶5) was used as mobile phase, the detection wavelength was set at 254 nm, the flow rate was 7 mL/min, the injection volume was 1.2 mL(the loading amount was about 1.728 mg), and the camptothecin(CPT) was separated and purified at room temperature. And the purification rate of CPT was 88.08%, compared with the crude extract, the purity increased by 45.78 percentage points.

Key words: rosin, stationary phase, preparation column, camptothecin, preparative liquid chromatography

CLC Number:

TQ35

Fengmei YI, Wenbo XIE, Hao LI, Lei ZENG, Wen LI, Fuhou LEI. Preparation of Core-shell SiO₂@Rosin-based Polymer High Performance Liquid Preparation Column and Purification of Camptothecin[J]. Chemistry and Industry of Forest Products, 2021, 41(6): 67-75.

Figures/Tables 12

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References 30

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样品 sample	比表面积/(m²·g^-1) specific surface area	平均孔径/nm average pore size	孔体积/(cm³·g^-1) pore volume
活化硅胶 activated silica gels	451.25	6.67	0.94
核壳型固定相 core-shell stationary phase	334.53	5.97	0.65

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Preparation of Core-shell SiO₂@Rosin-based Polymer High Performance Liquid Preparation Column and Purification of Camptothecin

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Preparation of Core-shell SiO2@Rosin-based Polymer High Performance Liquid Preparation Column and Purification of Camptothecin

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Preparation of Core-shell SiO₂@Rosin-based Polymer High Performance Liquid Preparation Column and Purification of Camptothecin