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A kind of preparation method of silica gel matrix hplc filler

A silica gel matrix and silica gel technology, applied in separation methods, chemical instruments and methods, and other chemical processes, can solve the problems of unstable silicon-oxygen bonds, bonded chain removal and breakage, etc., achieve good symmetry, reduce adsorption, The effect of high column efficiency

Active Publication Date: 2021-09-21
中科微分科技发展(北京)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In the prior art, the silicon-oxygen bond in the bonded silica gel filler of the silica gel matrix is ​​unstable when the acidity is strong, and the bonded chain is easily removed and broken.

Method used

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  • A kind of preparation method of silica gel matrix hplc filler
  • A kind of preparation method of silica gel matrix hplc filler
  • A kind of preparation method of silica gel matrix hplc filler

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] A kind of preparation method of silica gel matrix HPLC filler

[0048] S1: Mix formula 1 (1 mol) and formula 2 (2.1 mol) in THF (the mass ratio of volume and formula 1 is 8ml / g), add NaI (0.15 mol) and NaI 2 CO 3 (2mol), react at 25°C for 12h. After the reaction was completed, the reaction solution was filtered, water was added to the filtrate for extraction, the organic phase was collected, concentrated and dried to obtain formula 3 (0.85mol);

[0049] S2: Dissolve formula 3 (0.5 mol) in THF: water = 10:1 mixed solvent (volume dosage is 20ml / g with the mass ratio of formula 3), use hydrochloric acid to adjust the pH to 2, then add formaldehyde water dropwise (CH 2 O 2.5mol) solution, the temperature was raised to 50° C., sealed and reacted for 12 hours to obtain formula 4;

[0050] Use GPC (gel permeation chromatography) to measure the Mw (weight average molecular weight)=1.32x10 of formula 4 4 .

[0051] S3: Add silica gel (0.3 times the weight of formula 3) to ...

Embodiment 2

[0053] A kind of preparation method of silica gel matrix HPLC filler

[0054] S1: Mix Formula 1 (1mol) and Formula 2 (2.0mol) in THF (volume ratio of 10ml / g to Formula 1), add KI (0.1mol) and NaHCO 3 (2.5mol), react at 25°C for 12h. After the reaction was completed, the reaction solution was filtered, water was added to the filtrate for extraction, the organic phase was collected, concentrated and dried to obtain formula 3 (0.82mol);

[0055] S2: Dissolve Formula 3 (0.5mol) in a mixed solvent of 1,4-dioxane: water = 10:1 (the mass ratio of volume and Formula 3 is 15ml / g), and use hydrochloric acid to adjust the pH to 4, followed by dropwise addition of formalin (CH 2 (2mol) solution, the temperature was raised to 60° C., and the reaction was sealed for 12 hours to obtain formula 4;

[0056] Use GPC (gel permeation chromatography) to measure the Mw (weight average molecular weight)=1.28x10 of formula 4 4 .

[0057] S3: Add silica gel (0.5 times the weight of Formula 3) to ...

Embodiment 3

[0059] A kind of preparation method of silica gel matrix HPLC filler

[0060] S1: Mix Formula 1 (1mol) and Formula 2 (2.2mol) in THF (volume ratio of 10ml / g to Formula 1), add NaI (0.2mol) and KHCO 3 (2.5mol), react at 25°C for 12h. After the reaction was completed, the reaction solution was filtered, water was added to the filtrate for extraction, the organic phase was collected, concentrated and dried to obtain formula 3 (0.87mol);

[0061] S2: Dissolve formula 3 (0.5mol) in THF: water = 5:1 mixed solvent (volume dosage is 20ml / g with the mass ratio of formula 3), use hydrochloric acid to adjust the pH to 3, then add formaldehyde water dropwise (CH 2 (03mol) solution, the temperature was raised to 50° C., and the reaction was sealed for 12 hours to obtain formula 4;

[0062] Use GPC (gel permeation chromatography) to measure the Mw (weight average molecular weight)=1.41x10 of formula 4 4 .

[0063] S3: Add silica gel (0.4 times the weight of Formula 3) to the system aft...

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Abstract

The invention relates to the field of chemical analysis instruments, in particular to a method for preparing a silica gel-based HPLC filler. A macromolecule has been prepared, the macromolecule has C18 hydrophobic long chain as a side chain, and has a hydrophilic amide bond main chain at the same time. In the preparation method of the present invention, the hydrophilic amide in the obtained macromolecule The functional group can have a good affinity with the silanol on the surface of silica gel, and at the same time, by utilizing the adsorption of silica gel, the polymer prepared by the present invention can be tightly bound to the surface of silica gel without bonding. At this time, the C18 hydrophobic long chain It is exposed on the outside, which has the performance of C18 reversed-phase bonded packing, and at the same time avoids the influence of the silanol bonded to silica gel on the market on the alkaline analyte or separation.

Description

technical field [0001] The invention relates to the field of chemical analysis instruments, in particular to a method for preparing a silica gel-based HPLC filler. Background technique [0002] HPLC, High Performance Liquid Chromatography, Chinese name: High Performance Liquid Chromatography. It is a separation and analysis technique used in chemistry, medicine, industry, agronomy, commodity inspection and legal inspection and other disciplines. It can be divided into "high pressure infusion pump", "chromatographic column", "sampler", "detector", "fraction collector" and "data acquisition and processing system". The chromatographic column is the basis for separating mixed substances. [0003] Commonly used fillers can be divided into three categories according to different substrates: inorganic substrates, organic substrates and organic-inorganic composite matrix fillers. Among them, the inorganic matrix is ​​mainly silica gel, which generally has the advantages of high c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J20/30B01D15/26
CPCB01D15/265B01J20/22
Inventor 郭保胜
Owner 中科微分科技发展(北京)有限公司