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Hydrophilic chromatographic stationary phase with copolymer brush grafted on POSS silica gel as well as preparation method and application thereof

A graft copolymer and hydrophilic chromatography technology is applied in the field of hydrophilic chromatography stationary phase and its preparation, and achieves the effects of good separation performance, improved density and improved separation ability

Active Publication Date: 2021-12-10
BEIFANG UNIV OF NATITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the currently reported HILIC stationary phase only grafts a monomer to form a hydrophilic homopolymer brush on the surface of the stationary phase to synthesize the HILIC stationary phase.

Method used

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  • Hydrophilic chromatographic stationary phase with copolymer brush grafted on POSS silica gel as well as preparation method and application thereof
  • Hydrophilic chromatographic stationary phase with copolymer brush grafted on POSS silica gel as well as preparation method and application thereof
  • Hydrophilic chromatographic stationary phase with copolymer brush grafted on POSS silica gel as well as preparation method and application thereof

Examples

Experimental program
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Embodiment 1

[0036] The purpose of this embodiment is to provide a kind of preparation method of the hydrophilic chromatographic stationary phase of graft copolymer brush on POSS silica gel, as figure 1 Shown, specifically prepare according to the following steps:

[0037] S1. Put 3.0 g of silica gel in a three-necked bottle of 40 ml of 2mol / L hydrochloric acid, soak it at 120°C for 12 hours, wash it with deionized water, and dry it in vacuum at 120°C for 8 hours to obtain activated silica gel, which is denoted as Sil.

[0038] S2. Add 40ml of reflux-treated dry toluene into a 250ml three-necked bottle, add 3.0g Sil, and add 1.2ml of trimethoxychlorosilane dropwise under nitrogen protection, then reflux and stir at 110°C for 24 hours under nitrogen protection, and then The reaction solution was cooled to room temperature, filtered to remove the remaining solution, washed repeatedly with toluene and methanol three times, and vacuum-dried at 110°C for 6 hours to obtain chlorine-modified sili...

Embodiment 2

[0046] The purpose of this embodiment is to provide a kind of preparation method of the hydrophilic chromatographic stationary phase of graft copolymer brush on POSS silica gel, specifically prepare according to the following steps:

[0047] S1. Put 4.0 g of silica gel in a three-necked bottle of 40 ml of 4mol / L hydrochloric acid, soak it at 110°C for 9 hours, wash it with deionized water, and dry it in vacuum at 110°C for 10 hours to obtain activated silica gel, which is denoted as Sil.

[0048] S2. Add 40ml of reflux-treated dry toluene into a 250ml three-necked bottle, add 4.0g Sil, and add 1.5ml of trimethoxychlorosilane dropwise under nitrogen protection, then reflux and stir at 120°C for 20h under nitrogen protection, and then The reaction solution was cooled to room temperature, filtered to remove the remaining solution, washed repeatedly with toluene and methanol three times, and vacuum-dried at 120°C for 6 hours to obtain chlorine-modified silica gel, which was denoted...

Embodiment 3

[0053] The purpose of this embodiment is to provide a kind of preparation method of the hydrophilic chromatographic stationary phase of graft copolymer brush on POSS silica gel, specifically prepare according to the following steps:

[0054] S1. Put 3.5g of silica gel in a three-necked bottle of 40ml of 6mol / L hydrochloric acid, soak it in 115°C for 6h, wash it with deionized water, and dry it in vacuum at 115°C for 9h to obtain activated silica gel, which is denoted as Sil.

[0055] S2. Add 40ml of reflux-treated dry toluene into a 250ml three-necked bottle, add 3.5g of Sil, and add 1.3ml of trimethoxychlorosilane dropwise under nitrogen protection, then reflux and stir at 115°C for 22 hours under nitrogen protection, and then The reaction solution was cooled to room temperature, filtered to remove the remaining solution, washed repeatedly with toluene and methanol four times, and vacuum-dried at 115°C for 9 hours to obtain chlorine-modified silica gel, which was designated as...

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Abstract

The invention discloses a hydrophilic chromatographic stationary phase with a copolymer brush grafted on POSS silica gel as well as a preparation method and an application thereof, and belongs to the technical field of hydrophilic chromatographic stationary phases. The preparation method comprises the following steps: acidizing silica gel to obtain activated silica gel, carrying out a silane coupling reaction on the activated silica gel and trimethoxychlorosilane in a protective gas atmosphere to obtain chlorine modified silica gel, and carrying out a substitution reaction on the chlorine modified silica gel and octa-amino-POSS to obtain POSS modified silica gel; performing a coupling reaction on 2-bromine-isobutyryl bromide and the POSS modified silica gel, and obtaining bromine-containing silica gel; by taking POSS as a raw material, taking bromine-containing silica gel as an initiator and taking acrylamide and methacrylic acid-2, 3-dihydroxypropyl ester as comonomers, carrying out surface-initiated atom transfer radical polymerization reaction to obtain a hydrophilic chromatographic stationary phase with a copolymer brush grafted on the POSS silica gel, introducing two monomers with different polar groups into the stationary phase, so that the strong retention of hydrophilic interaction chromatography is facilitated.

Description

technical field [0001] The invention relates to the technical field of hydrophilic chromatographic stationary phases, in particular to a hydrophilic chromatographic stationary phase grafted with copolymer brushes on POSS silica gel and its preparation method and application. Background technique [0002] High-performance liquid chromatography (HPLC) has penetrated into almost every field. At present, reversed-phase liquid chromatography (RPLC) has been widely used to separate various substances. But for the separation of increasingly complex biological samples, the retention of these polar substances on RPLC is weak, resulting in poor separation effect. In order to solve the separation requirements of biological samples, Hydrophilic interaction liquid chromatography (HILIC) was born as a substitute application of RPLC. More importantly, HILIC often uses organic-rich mobile phases. Compared with RPLC, HILIC mobile phases with higher organic content are more compatible with ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/12C08F220/56C08F220/20B01D15/10
CPCC08F283/12B01D15/10C08F2438/01C08F220/56C08F220/20
Inventor 卜春苗李妍刘斌
Owner BEIFANG UNIV OF NATITIES
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