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Preparation method of full porous silica microparticle chiral chromatography packing

A silica gel microsphere and chiral chromatography technology is applied in the field of preparation of porous microsphere chromatographic fillers, which can solve the problems of different sizes and poor shape of microspheres, and achieve the effects of simple steps, good spheroidization and high porosity.

Active Publication Date: 2016-07-13
ZHEJIANG UNIV
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  • Abstract
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  • Claims
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Problems solved by technology

It has the disadvantages that the prepared microspheres are poorly shaped and have different sizes

Method used

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  • Preparation method of full porous silica microparticle chiral chromatography packing
  • Preparation method of full porous silica microparticle chiral chromatography packing
  • Preparation method of full porous silica microparticle chiral chromatography packing

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Embodiment 1

[0036] Example 1. A preparation method of a fully porous silica gel microsphere chiral chromatographic packing, followed by the following steps:

[0037] 1) Add 50g of tetraethoxysilane to 100g of absolute ethanol, stir in a three-necked flask at 30°C for 30 minutes, then add 1.5g of cyclohexane as a stabilizer and polyethylene as a porogen Alcohol (its molecular weight is 400) 7.5g, after mixing well, add 0.1g / ml hydrochloric acid solution to control the pH at 2, continue to stir for 60 minutes and raise the temperature to 90°C to evaporate the absolute ethanol, and then pass it in Argon, keep the temperature (90°C) and stir for 24 hours under the protection of argon, and finally raise the temperature to 140°C to evaporate the remaining liquid organics to obtain polyethoxysilane;

[0038] 2). Mix 30g of the polyethoxysilane obtained in step 1) with 30g of deionized water and 60g of absolute ethanol, add 0.1g / ml of hydrochloric acid to control the pH of the solution at 2, and mix t...

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Abstract

The invention discloses a preparation method of a full porous silica microparticle chiral chromatography packing. The method comprises the following steps: uniformly mixing tetraethoxysilane, absolute ethyl alcohol, a stabilizer and a pore-foaming agent, and then rising the temperature under the protection of inert gas to perform reaction, so as to obtain polyethoxysiloxane; uniformly mixing the polyethoxysiloxane, deionized water and absolute ethyl alcohol, and then sequentially performing gel coagulation, ageing, washing, drying and heat treatment, so as to obtain porous gel microparticles; packing the gel microparticles into 0.1g / ml hydrochloric acid, so as to be subjected to backflow activization, then putting the gel microparticles into a 0.1g / ml amylase-tris(3,5-dimethylphenylcarbamate) solution, stirring the gel microparticles for 5 to 7 hours, performing modification treatment on the gel microparticles, and finally performing drying, so as to obtain the full porous silica microparticle chiral chromatography packing.

Description

Technical field [0001] The invention belongs to the preparation field of porous microsphere chromatographic fillers, and specifically relates to a preparation method of porous silica microsphere chiral chromatographic fillers. Background technique [0002] Chirality means that the substance itself cannot completely overlap with its mirror image. It is one of the essential attributes of nature. Chirality is very common in drug synthesis. Most chiral drugs contain one or more chiral centers, so they contain a pair of And more than one pair of enantiomers. However, different chiral enantiomers often exhibit different drug activities, and some chiral isomers even contain toxicity, so it is very important for the separation of chiral drugs. Nowadays, with the deepening of the basic research of chromatographic theory and the improvement of chromatographic technology, and due to the short operating time of high performance liquid chromatography and the high sample load, it is conducive...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/30B01J20/28B01J20/286B01D15/08
CPCB01D15/08B01J20/28021B01J20/28061B01J20/28078B01J20/28088B01J20/286B01J2220/46B01J2220/54
Inventor 郭兴忠王睿赵岳星杨辉
Owner ZHEJIANG UNIV
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