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Chiral chromatographic stationary phase of polymer-coated silica and preparation method thereof

A chiral chromatography and polymer technology, applied in the field of material chemistry, can solve problems such as clogged injection port or column inlet, difficulty in reaching ideal concentration, poor solubility of inclusion complexes, etc., and achieves mild conditions and chiral separation effect Good, high column efficiency

Inactive Publication Date: 2013-04-03
江苏易谱恒科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the method of using chiral mobile phase additives also has many shortcomings that are difficult to overcome, which limits its application, such as: (1) the solubility of cyclodextrin in the mobile phase is low, and it is difficult to reach the desired concentration; (2) the formed package The solubility of the solid may become poor, and it will precipitate and block the inlet or column inlet; (3) the method with mobile phase additives has relatively small selectivity

Method used

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  • Chiral chromatographic stationary phase of polymer-coated silica and preparation method thereof
  • Chiral chromatographic stationary phase of polymer-coated silica and preparation method thereof
  • Chiral chromatographic stationary phase of polymer-coated silica and preparation method thereof

Examples

Experimental program
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Embodiment 1

[0030] The preparation of the silica gel matrix of embodiment 1 coating polymer

[0031] Initiate the ATRP coated polymer layer on the surface of silica gel: take a round-bottomed three-necked flask, add successively 2.1 grams of silica gel with surface grafted ATRP initiator, 1.09 milliliters (7.18 mmol) of methyl butynyl methacrylate, and 1.00 ml of divinylbenzene milliliter (7.18mmol) and 30 milliliters of cyclohexanone, logical N 2 After 10 minutes, add 0.4475 grams (2.87mmol) of 2,2'-bipyridine and CuBr 0.2068 grams (1.44mmol), N 2 Under protection, react at 110°C for 4 hours. The density of bromine on the surface of silica gel is 0.9 micromole per square meter. After the reaction is completed, pour the reaction mixture suspension into absolute ethanol, stop the reaction, wash away the copper ions adsorbed on the surface of the silicon ball with saturated EDTA-2Na aqueous solution, then wash away the unreacted matter with acetone, and dry in vacuum , to obtain a polym...

Embodiment 2

[0032] The preparation of the silica gel matrix of embodiment 2 coating polymer

[0033] The difference from Example 1 is that the amount of each raw material is 2.1 grams of silica gel with surface-grafted ATRP initiator, 1.26 mmol of cuprous bromide, 2.31 mmol of 2,2'-bipyridine, and 6.3 mmol of methyl butynyl methacrylate. mmol, divinylbenzene 6.3 mmol. The polymerization time was 3 hours and the temperature was 105°C. Silicone matrices coated with polymers can likewise be produced.

Embodiment 3

[0034] The preparation of the silica gel matrix of embodiment 3 coating polymer

[0035] The difference from Example 1 is that the amount of each raw material is 2.1 grams of silica gel with surface-grafted ATRP initiator, 1.47 mmol of cuprous bromide, 3.15 mmol of 2,2'-bipyridine, and 8.4 grams of methyl butynyl methacrylate. mmol, divinylbenzene 8.4 mmol. The polymerization time was 5 hours and the temperature was 115°C. Silicone matrices coated with polymers can likewise be produced.

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Abstract

The invention discloses a chiral chromatographic stationary phase of polymer-coated silica and a preparation method thereof, belonging to the technical field of the material chemistry. The chromatographic stationary phase has the structure that a grafted azide group is grafted on the surface of a silica microsphere with a cyclodextrin polymer layer. The preparation method adopted by the chiral chromatographic stationary phase of the polymer-coated silica comprises the steps of coating a polymer layer containing alkynyl on the surface of the silica microsphere by adopting an atom transfer redical polymerization, taking methacrylic acid-methyl-butyne alcohol ester as an monomer, taking divinylbenzene as a cross-linking agent, and then clicking chemically grafted cyclodextrin containing the azide group to obtain the chiral chromatographic stationary phase. The chiral chromatographic stationary phase of the polymer-coated silica has the advantages that the polymer coating layer in the stationary phase has favorable controllability and strong solvent resistance, and also has the advantages of high column efficiency, good chiral separation effect and wide application scope.

Description

technical field [0001] The invention relates to a preparation method of a chiral separation stationary phase, in particular to a preparation method of a silica gel matrix surface coated with a polymer layer, and belongs to the technical field of material chemistry. Background technique [0002] For high performance liquid chromatography, cyclodextrins can not only be bonded to stationary phase supports, but also used as mobile phase additives. In terms of application, chiral mobile phase additives have certain advantages. This method is technically easy to implement, and chiral separation can be achieved on conventional chromatographic columns. However, the method of using chiral mobile phase additives also has many shortcomings that are difficult to overcome, which limits its application, such as: (1) the solubility of cyclodextrin in the mobile phase is low, and it is difficult to reach the desired concentration; (2) the formed package The solubility of the solid may beco...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/29B01J20/30
Inventor 姜久英王海燕周瑾丹
Owner 江苏易谱恒科技有限公司
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