Chromatographic separation material based on copolymerization on silica gel surface and preparation thereof

A technology of copolymerization reaction and chromatographic separation, which is applied in the field of silica gel matrix bonded "non-polar/polar copolymerization stationary phase" and its preparation, can solve the problems of fixed spatial position and difficult regulation, and achieve large bonding amount and improved Selective, structurally novel effects

Active Publication Date: 2013-01-02
浙江华谱新创科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the spatial positions of polar groups and non-polar ligands are relatively fixed, making it difficult to regulate
However, currently no technology exists to prepare polar reversed-phase chromatography stationary phases using this method

Method used

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  • Chromatographic separation material based on copolymerization on silica gel surface and preparation thereof
  • Chromatographic separation material based on copolymerization on silica gel surface and preparation thereof
  • Chromatographic separation material based on copolymerization on silica gel surface and preparation thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Weigh 10g spherical silica gel (particle size is 5μm, pore size is 10nm, specific surface area is 305m 2 / g), placed in a 250mL glass flask, added 150mL of 10% hydrochloric acid solution by volume, heated to reflux for 12 hours, cooled to room temperature, filtered, washed with water until neutral, and dried at 150°C for 24 hours. The dried silica gel was placed in a 150 mL three-neck glass bottle, and nitrogen gas with a relative humidity of 50% was continuously introduced for 48 hours to obtain 10.5 g of hydrated silica gel. Under the condition of passing through dry nitrogen, add 80mL of dry n-hexane to the hydrated silica gel, stir well, then add 18mmol (7.2mL) of octadecyltrichlorosilane and 6mmol (0.9mL) of 3-chloropropyl The trichlorosilane mixture was stirred at room temperature for 24 hours. The reaction system was filtered, washed successively with toluene, dichloromethane, methanol, water, tetrahydrofuran, and methanol, and the product was dried at 80° C. fo...

Embodiment 2

[0026] Its preparation method is: weigh 10g of spherical silica gel (particle size is 3μm, pore size is 12nm, specific surface area is 290m 2 / g), placed in a 250mL glass flask, added 100mL of 38% hydrochloric acid solution, heated to reflux for 2 hours, cooled to room temperature, filtered, washed with water until neutral, and dried at 120°C for 24 hours. The dried silica gel was placed in a 150 mL three-necked glass bottle, and nitrogen gas with a relative humidity of 60% was continuously introduced for 24 hours to obtain 10.3 g of hydrated silica gel. Under the condition of blowing dry nitrogen, add 80mL of dry toluene to the hydrated silica gel, stir well, then add 16mmol (6.4mL) octadecyltrichlorosilane and 8mmol (1.9mL) 3-cyanopropyltrichlorosilane dropwise. Chlorosilane mixture was stirred and reacted at 80°C for 24 hours. The reaction system was filtered, washed successively with toluene, dichloromethane, methanol, water, tetrahydrofuran, and methanol, and the product...

Embodiment 3

[0029] Weigh 10g spherical silica gel (particle size is 5μm, pore size is 10nm, specific surface area is 305m 2 / g), placed in a 250mL glass flask, added 150mL of 10% hydrochloric acid solution, heated to reflux for 12 hours, cooled to room temperature, filtered, washed with water until neutral, and dried at 120°C for 24 hours. The dried silica gel was placed in a 150 mL three-necked glass bottle, and nitrogen gas with a relative humidity of 30% was continuously introduced for 72 hours to obtain 10.6 g of hydrated silica gel. Under the condition of blowing dry nitrogen, add 100mL dry n-pentane to the hydrated silica gel, stir well, then add 16mmol (6.4mL) octadecyltrichlorosilane and 8mmol (1.4mL) 3-aminopropane dropwise Base trimethoxysilane mixture, stirred at room temperature for 24 hours. The reaction system was filtered, washed successively with toluene, dichloromethane, methanol, water, tetrahydrofuran, and methanol, and the product was dried at 80° C. for 12 hours to o...

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Abstract

A separation material based on silica gel substrate and preparation method thereof are provided. The separation material based on silica gel substrate is obtained by copolymerizing two or more silane reagents on the silica gel surface to form "non-polar / polar copolymerized stationary phase" and has the following formula, wherein NP denotes non-polar groups, which comprise C1-30 n-alkane groups, phenyl, and so on; P denotes polar groups, which comprise C1-12 n-alkane groups jointing with Cl, Br, CN, amino group, benzenesulfonic group, sulfonic group, carboxyl group, quaternary ammonium group, alcohol group, and so on. The preparation method of the above mentioned separation material comprises the following steps: acidification preprocessing of silica gel, hydrating, copolymerizing a mixture of non-polar silane reagent and polar silane reagent on the hydrated silica gel surface, filtering, washing, drying, and so on. The separation material of the present invention has both non-polar groups and polar groups, which can provide hydrophobic applied force and several kinds of polar applied forces, and thereby improve greatly the selectivity of separation and enrichment. The separation material obtained through the preparation method of the present invention has merits such as uniform and stable bonding groups on the surface, larger bonding amount and so on, and can be applied to liquid chromatogram chromatography and solid phase extraction.

Description

technical field [0001] The invention relates to a chromatographic separation material, specifically a silica gel substrate-bonded "nonpolar / polar copolymerization stationary phase" based on silica gel surface copolymerization reaction and a preparation method thereof. Background technique [0002] Reversed-phase high-performance liquid chromatography is the most widely used separation and analysis technique. Silica-based octadecyl-bonded stationary phase is the most commonly used separation material for reversed-phase chromatography. However, the octadecyl stationary phase can only provide a single hydrophobic force, and has poor retention and separation selectivity for polar compounds. Therefore, on the basis of conventional reversed-phase stationary phases, polar groups are introduced, and bonded stationary phases that can provide both hydrophobic and polar interaction forces are developed to supplement the polar selectivity in the reversed-phase chromatography separation...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01J20/287B01J20/30
CPCB01J20/3244B01J20/3285B01J20/3246B01J20/328B01J20/3272B01J20/286B01J20/3257B01D15/32
Inventor 郭志谋梁图金高娃梁鑫淼
Owner 浙江华谱新创科技有限公司
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