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[0003] The current method for preparing a bonded stationary phase chiral chromatographic column is to first prepare a bonded stationary phase, and then pack the stationary phase into a chiral column. The preparation steps are numerous, the time is long, and the operation is complicated, as disclosed in Chinese patent CN 100387333C Preparation
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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Embodiment 1
[0033] 1) Treatment of silica gel
[0034] Take 10 grams of silica gel (average particle diameter about 5 microns, pore diameter about 30 nanometers) treated and dried with 20% hydrochloric acid in a conventional activation manner, add 50 milliliters of toluene, and then add 10 milliliters of γ-methacryloyloxy Propyltriethoxysilane was heated at 105°C under nitrogen protection and reacted for 12 hours. The reaction product was washed with toluene and ethanol in sequence and dried.
[0035] 2) Bonded silica gel column packing
[0036] Take 2.1 grams of the above-mentioned silanized silica gel with unsaturated double bonds, and pack it into a column by a slurry method to prepare a Φ4.6×150 mm liquid chromatography column.
[0037] 3) Preparation of polysaccharide derivatives
[0038] Take 3 grams of cellulose, add 150 milliliters of pyridine, add 1 gram of 3-ethoxyacryloyl chloride, react at 80 degrees Celsius for 5 hours under nitrogen protection, and then add 20 milliliters ...
Embodiment 2
[0043] 1) Treatment of silica gel
[0044] Take 10 grams of silica gel (average particle diameter of about 5 microns and pore diameter of about 30 nanometers) treated and dried with 20% hydrochloric acid in a conventional activation manner, add 50 milliliters of toluene, and then add 8 milliliters of vinyltriethoxysilane, Heated at 105°C under nitrogen protection, and reacted for 12 hours. The reaction product was washed with toluene and ethanol in sequence and dried.
[0045] 2) Bonded silica gel column packing
[0046] Take 2.1 grams of the above-mentioned silanized silica gel with unsaturated double bonds, and pack it into a column by a slurry method to prepare a Φ4.6×150 mm liquid chromatography column.
[0047] 3) Preparation of polysaccharide derivatives
[0048] Take 3 grams of amylose, add 150 milliliters of pyridine, add 1 gram of 3-ethoxyacryloyl chloride, react at 80 degrees Celsius for 5 hours under nitrogen protection, and then add 20 milliliters of 3,5-dimethyl...
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Abstract
The present invention provides a bonding type stationary phase chiral chromatographic column preparation method, which comprises: preparing a silica gel bonded with the unsaturated double bond, loading the silica gel into a chiral chromatographic column, preparing a polysaccharide derivative bonded with the unsaturated double bond, injecting the polysaccharide derivative into the chiral chromatographic column in a solution form so as to make the polysaccharide derivative be uniformly adsorbed on the silica gel surface, and injecting an initiator solution into the chiral chromatographic column, such that the unsaturated double bond of the silica gel and the unsaturated double bond of the polysaccharide derivative are subjected to a polymerization reaction so as to form the bonding type stationary phase. According to the preparation method of the present invention, the adsorption step and the bonding step in the conventional preparation method are completed in the chromatographic column, such that the steps and the process are simplified, characteristics of simpleness, rapidness and high efficiency are provided, the prepared chiral chromatographic column stationary phase is uniform, the bonding type stationary phase chiral chromatographic column can be used for a variety of strong polar 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 method for preparing a bonded stationary phase chiral chromatographic column is...
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