Preparation method of bonding type stationary phase chiral chromatographic column

Abstract

The invention provides a preparation method of a bonding type stationary phase chiral chromatographic column. The method comprises the following steps: firstly preparing silica gel bonded with unsaturated double bond and filling into a chiral chromatographic column, then preparing a polysaccharide derivative compound bonded with unsaturated double bond, injecting the polysaccharide derivative compound into the chiral chromatographic column in a solution form to enable the polysaccharide derivative compound to be evenly adsorbed to the surface of the silica gel, and then injecting an initiator solution to the chiral chromatographic column, so that the unsaturated double bond of the silica gel and the unsaturated double bond of the polysaccharide derivative compound generate polymerization reaction to form a bonding type stationary phase. According to the preparation method disclosed by the invention, steps of adsorbing and bonding in conventional preparation methods are completed in the chromatographic column, so that the steps and the process are simplified; the preparation method has the characteristics of being simple, quick and high in efficiency; the stationary phase of the prepared chiral chromatographic column is uniform and can be applied to multiple strong-polarity mobile phases; the column efficiency is high and the separation effect is good.

Description

technical field [0001] The invention relates to the field of chiral chromatographic columns, in particular to a preparation method of a bonded stationary phase chiral chromatographic column. Background technique [0002] Polysaccharide chiral stationary phases have shown great advantages in the separation and preparation of chiral enantiomers, and have broad application prospects. At present, most of the commercialized chiral stationary phases of polysaccharide derivatives adopt the method of physical coating to immobilize the polysaccharide derivatives on the surface of silica gel, so there is a problem of chiral stationary phase loss, and they are not resistant to most of the stronger ones. Polar solvents bring many restrictions to practical use. In response to these problems, bonded polysaccharide chiral stationary phases emerged to overcome the above-mentioned problems. [0003] The current preparation method of the bonded stationary phase chiral chromatographic column...

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Problems solved by technology

[0003] The current preparation method of the bonded stationary phase chiral chromatographic column is to prepare the bonded stationary phase first, and then pack the stationary phase into the chiral column. The preparation steps are numerous, the time is long, and the operation is complicated, such as the preparation disclosed in Chinese patent CN100387333C method

In the preparation process of the stationary phase, the polysaccharide derivative bonded with unsaturated double bonds is first coated on the surface of the silica gel. The coating thickness is difficult to control during the coating process, and the coating thickness of the polysaccharide derivative coated on the silica gel is uneven. The particle size and specific surface area of ​​the bonded silica gel vary greatly and are uneven. This phenomenon is more prominent in the small particle size silica gel filler, and the resulting chiral chromatography column stationary phase is not uniform. In addition, the polysaccharide derivative coating Thicker silica gel fillers are prone to deformation or falling off during filling, and these phenomena seriously affect the column efficiency and separation ability of chiral chromatographic columns

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