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Novel silica gel matrix surface modification method and application of surface-modified silica gel matrix

A technology of surface modification and silica gel matrix, which is applied in the field of chromatographic separation. It can solve the problems of low bond and efficiency and non-specificity of silanol materials, and achieve high bond and density, increase bond and density, and high-efficiency separation.

Active Publication Date: 2019-06-11
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the problems of traditional silica gel bonds and existing bonds and low efficiency, and the non-specificity of the material silanol to the sample, a new method for surface modification of silica gel substrates is proposed.

Method used

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  • Novel silica gel matrix surface modification method and application of surface-modified silica gel matrix
  • Novel silica gel matrix surface modification method and application of surface-modified silica gel matrix
  • Novel silica gel matrix surface modification method and application of surface-modified silica gel matrix

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1. Preparation of reversed-phase C18 chromatography packing material

[0027] like figure 1 As shown, it is prepared according to the following process:

[0028] (1) Surface activation of silica gel: Disperse 1 g of silica gel in 1M hydrochloric acid, reflux at constant temperature for 12 hours under stirring; then wash with distilled water until neutral; finally dry at 70°C.

[0029] (2) High-density bonding of silylating agents: disperse the activated silica gel in 50% N-propenyl-aza-2,2-dimethoxysilapentane in dichloromethane solution (v / v); At a constant temperature of 25°C, the stirring time was 2h.

[0030] (3) Click reaction: Accurately weigh 20 mg of silica gel, 3 mg of AIBN, 20 mg of mercaptooctadecyl, and 750 μL of ethanol, mix well, and react at a constant temperature of 60° C. for 12 hours. After the reaction is completed, rinse with ethanol for 1 h, filter, and dry at 50°C to obtain a modified reversed-phase C18 chromatographic filler. 2. The effect of ...

Embodiment 2

[0039] like figure 1 As shown, the reversed-phase C18 chromatographic filler was prepared according to the following process:

[0040] (1) Surface activation of silica gel: Disperse silica gel in 1M sulfuric acid, reflux at constant temperature for 12 hours under stirring; then wash with distilled water until neutral; finally dry at 70°C.

[0041] (2) High-density bonding of silylating reagents: disperse the activated silica gel in 50% N-propenyl-aza-2,2-dimethoxysilapentane in dichloromethane solution (v / v); Stir for a certain period of time at a constant temperature of 25°C.

[0042] (3) Click reaction: Accurately weigh 20mg of silica gel, 3mg of AIBN, 20mg of HSC 18 , 750 μL ethanol, after mixing evenly, react at a constant temperature of 60°C for 12h. After the reaction was completed, wash with ethanol for 1 h.

[0043] The chromatographic filler prepared by the above process has similar bond and efficiency to the material prepared in Example 1, and the zeta potential ...

Embodiment 3

[0045] like figure 1 As shown, the reversed-phase C18 chromatographic filler was prepared according to the following process:

[0046](1) Surface activation of silica gel: Disperse silica gel in 1M hydrochloric acid, reflux at constant temperature for 12 hours under stirring; then wash with distilled water until neutral; finally dry at 70°C.

[0047] (2) High-density bonding of silylating reagents: disperse the activated silica gel in 30% N-propenyl-aza-2,2-dimethoxysilapentane in dichloromethane solution (v / v); Stir for a certain period of time at a constant temperature of 25°C.

[0048] (3) Click reaction: Accurately weigh 20mg of silica gel, 3mg of AIBN, 20mg of HSC 18 , 750 μL ethanol, after mixing evenly, react at a constant temperature of 60°C for 12h. After the reaction was completed, wash with ethanol for 1 h.

[0049] The chromatographic filler prepared by the above process has similar bond and efficiency to the material prepared in Example 1, and the zeta potenti...

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Abstract

The invention discloses a novel silica gel matrix surface modification method and application of a surface-modified silica gel matrix. The novel silica gel matrix surface modification method is basedon a five-membered heterocyclic silylating reagent which has an unstable heterocyclic structure, and hydrolysis ring-opening is performed on the reagent and silanol groups, wherein the reactivity is high, and the bonding density is improved significantly; in addition, hydrophilic groups are formed by ring-opened heteroatoms, so that non-specific adsorption of analytes by unreacted silanol groups is avoided effectively. Compared with conventional chlorosilane modification, the novel silica gel matrix surface modification method has high bonding efficiency, mild reaction conditions and no cross-linking, the pore structure of silica gel can be ensured, and therefore the separation efficiency can be improved effectively by a chromatographic stationary phase prepared from the silica gel matrix;and the chromatographic stationary phase can be widely applied to separation of alkaline analytes and biological samples.

Description

technical field [0001] The invention relates to the field of functionalized materials and separation analysis, including chromatographic fillers with different hydrophobicities, a preparation method and an application in the field of chromatographic separation. Background technique [0002] Liquid chromatography technology is an important branch of analytical chemistry, which has become increasingly mature in recent years (Olives, A.I., Trends in Anal.Chem., 2015, 64:17-28; Fekete, S.Trends in Anal.Chem., 2014 , 63:2-13). The principle of separation is that the sample is dispersed in the mobile phase and driven by pressure or voltage to pass through the stationary phase. Based on the fact that different samples have different partition coefficients between the mobile phase and the stationary phase, resulting in different retention times, the separation of the samples is achieved. Due to its high efficiency and rapidity, this technique is widely used in different research fi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/287B01D15/32
Inventor 张丽华朱旭东梁玉杨开广李洋梁振张玉奎
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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