Silica gel chromatography packing and preparation method thereof

A silica gel chromatography and silica gel technology, applied in chemical instruments and methods, other chemical processes, etc., can solve problems such as strong electrostatic interaction, difficult elution of compounds, and reduced sensitivity, and achieve good compatibility, good stability, and excellent HILIC separation effect of ability

Active Publication Date: 2013-04-10
浙江月旭材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the filler has too strong electrostatic interaction between the compound and the stationary phase, the compound is not easy to elute, and needs to be adjusted with a high concentration of buffer salt, which will suppress the mass spectrometry signal and reduce the sensitivity.

Method used

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  • Silica gel chromatography packing and preparation method thereof
  • Silica gel chromatography packing and preparation method thereof
  • Silica gel chromatography packing and preparation method thereof

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preparation example Construction

[0037] The invention provides a method for preparing a hydrophilic silica gel chromatographic filler with zwitterions, comprising the following steps:

[0038] (1) Activate and pretreat the silica gel to obtain activated silica gel;

[0039] (2) Epoxy-modifying the activated silica gel to obtain epoxy-modified silica gel;

[0040] (3) introducing a tertiary amino group on the epoxy-modified silica gel to obtain a tertiary amino-modified silica gel;

[0041] (4) introducing a sulfonic acid group on the tertiary amino-modified silica gel to prepare the zwitterionic hydrophilic silica gel chromatographic filler.

[0042] Wherein the step (1) includes: washing the silica gel twice with distilled water, then soaking with hydrofluoric acid aqueous solution, then washing with distilled water until the pH value is neutral, finally washing with acetone and drying.

[0043] Wherein the step (2) comprises: using toluene as a solvent, after dissolving the activated silica gel evenly, addi...

Embodiment 1

[0048] Embodiment 1: Preparation of hydrophilic silica gel chromatography filler with zwitterions

[0049] (1) Add 20g of silica gel (5 μm, purchased from Daiso Co., Japan) into a 250mL reaction vessel, add 200mL of distilled water, stir for 30 minutes, filter, and repeat this step twice. Then add 160mL mass ratio of 0.08% hydrofluoric acid aqueous solution, stir for 24 hours, wash with distilled water until neutral, finally add 200mL acetone to wash, filter, and dry at 110°C for 12 hours to obtain activated silica gel;

[0050] (2) Weigh 20g of activated silica gel (5μm, ), placed in a 500mL reaction vessel; add 120mL toluene: add 20mL γ-(2,3-epoxypropoxy)propyltrimethoxysilane (Gelest, USA) to the reaction vessel, and stir under reflux at 97°C Reaction for 20-22 hours: wash the prepared packing with 400mL hot ultrapure water, 400mL hot THF / water (volume ratio 80:20), 400mL hot THF and 400mL hot acetonitrile, and filter to obtain epoxy group Modified silica gel;

[0051] ...

Embodiment 2

[0053] Embodiment 2: Preparation of hydrophilic silica gel chromatography filler with zwitterions

[0054] (1) Add 100g of silica gel to a 2L reaction vessel, add 200mL of distilled water, stir for 30 minutes, filter, and repeat this step twice. Then add 800mL mass ratio of 0.08% hydrofluoric acid aqueous solution, after stirring for 24 hours, wash with distilled water until neutral, finally add 200mL acetone to wash, filter, and dry at 110°C for 12 hours to obtain activated silica gel;

[0055] (2) Weigh 100g of activated silica gel (5μm, ), placed in a 3L reaction vessel; add 600mL of toluene: add 200mL of γ-(2,3-epoxypropoxy)propyltrimethoxysilane to the reaction vessel, reflux and stir at 97°C for 20-22 hours : Clean the prepared packing and filter with 2000mL hot ultrapure water, 2000mL hot THF / water (80:20), 2000mL hot THF and 2000mL hot acetonitrile successively, to obtain epoxy group modified silica gel;

[0056] (3) Add epoxy-modified silica gel prepared in step (2...

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Abstract

The invention provides a preparation method of zwitterionic hydrophilic silica gel chromatography packing. The preparation method comprises the following steps that (1) silica gel is subjected to activation pretreatment to prepare activated silica gel; (2) the activated silica gel is subjected to epoxidation modification to prepare epoxy modified silica gel; (3) tertiary amido is introduced onto the epoxy modified silica gel to prepare tertiary amido modified silica gel; and (4) sulfo is introduced onto the tertiary amido modified silica gel to prepare the zwitterionic hydrophilic silica gel chromatography packing. The prepared silica gel chromatography packing is small in electrostatic interaction and has a good absorption effect on an ionic or polar target object.

Description

technical field [0001] The invention relates to a silica gel chromatography filler, in particular to a hydrophilic silica gel chromatography filler with zwitterions and a preparation method thereof. Background technique [0002] In recent years, with the rapid development of research fields such as life sciences, modernization of traditional Chinese medicine, and environmental sciences, strongly polar, hydrophilic small molecules and basic drug molecules have become research hotspots in the fields of analytical chemistry and medicinal chemistry. However, it is often difficult to obtain effective separation of the above-mentioned target substances in liquid chromatography. On the one hand, the traditional reversed-phase chromatography (RPLC) has weak retention and separation ability for the above-mentioned target substances, which is due to the fact that the polar functional groups in the above-mentioned target substances are easy to form a "dipole moment interaction" with th...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/281B01J20/283B01J20/30
Inventor 薛昆鹏赵岳星姚立新
Owner 浙江月旭材料科技有限公司
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