Core-shell SiO2@rosin-based polymer microspheres and preparation method thereof

Abstract

The invention discloses core-shell SiO2@rosin-based polymer microspheres and a preparation method thereof. A rosin-based crosslinking agent, an acrylic monomer and a radical initiator are uniformly mixed, the mixture is uniformly applied to the surface of silica gel, the silica gel is placed in an aqueous phase for radical polymerization, and the core-shell SiO2@rosin-based polymer microspheres are obtained. The core-shell SiO2@rosin-based polymer microspheres have particle size distribution centralized in the range of 2-900 mu m, the mean pore size of 0.5-100 nm and the specific surface areaof 50-350 m<2> / g and have the characteristics of excellent degree of sphericity, uniform particle size, rich pore structure, high mechanical strength and high solvent tolerant degree, and a chromatographic column filled with the core-shell SiO2@rosin-based polymer microspheres as chromatographic packing especially has good separation effect on alkaloids, gastrodin and derivatives thereof.

Description

technical field [0001] The invention belongs to the technical field of high performance liquid chromatography, and in particular relates to a core-shell type SiO 2 @Rosin-based polymer microspheres and their preparation methods. Background technique [0002] As a separation method and technology, high-performance liquid chromatography has become more and more mature in recent years due to its advantages of high separation efficiency, high selectivity, high detection sensitivity, and fast analysis speed, and its application fields have gradually developed to the separation of pesticide residues and drugs. , food testing and other fields. As a place and tool for separation, a chromatographic column is the core of the entire HPLC system, and its performance directly determines the separation effect. The development of chromatographic packing determines the development of chromatographic columns. At present, according to the different matrix materials, chromatographic packing ...

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Problems solved by technology

[0003] At present, there are many studies on chromatographic fillers. For example, the invention patent application with application number 201710710292.1 discloses a weakly polar rosin-based polymer microsphere and its preparation method and application. It uses methyl methacrylate as a monomer, Using the rosin derivative propylene pimaric acid ethylene glycol acrylate as a cross-linking agent to prepare weakly polar rosin-based polymer microspheres and fill the chromatographic column with it, a good separation of gastrodin and its derivatives was achieved, but , the chromatographic column filled with the above-mentioned weakly polar rosin-based polymer microspheres has a narrow range of mobile phase selection, especially high sensitivity to water, which limits the further development of its excellent performance; such as Qin Feng, Chen Xiaoming, Liu Yueqi, etc. The cellulose-three (tetramethylbenzoate) derivatives with methacryloyl groups synthesized are bonded on the surface of silica gel with double bonds by polymerization to obtain a chiral stationary phase. , this method is difficult to control the polymerization process in the preparation process, so "agglomeration" is prone to occur, and the obtained microspheres have a wide particle size distribution and irregular shape; for another example, P.Li et al. EGMRA was used as a cross-linking agent to synthesize a paclitaxel molecularly imprinted polymer, which was used to fill a high-performance liquid chromatography column and realize the separation of paclitaxel and docetaxel. However, the molecularly imprinted polymer prepared by this method has high consumption costs and preparation The process is cumbersome, and the particle size distribution of the microspheres is wide, and the theoretical plate number of the chromatographic column obtained after filling is also low

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