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Embedded triazine ring amide silica gel stationary phase for liquid chromatograph and preparation method thereof

A technology of triazine cyclic amide and liquid chromatograph, applied in chemical instruments and methods, other chemical processes, etc., can solve problems such as not showing good separation effect, and achieve novel structure, stable bonding layer, good identification and The effect of separation performance

Active Publication Date: 2013-09-11
DALIAN ELITE ANALYTICAL INSTR +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of the above-mentioned imbedded polar functional group stationary phases are embedded with a single polar group, which has made progress in improving the tailing of basic compounds, but it is not suitable for the separation of complex sample systems such as structural analogs or isomers. Did not show good separation

Method used

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  • Embedded triazine ring amide silica gel stationary phase for liquid chromatograph and preparation method thereof
  • Embedded triazine ring amide silica gel stationary phase for liquid chromatograph and preparation method thereof
  • Embedded triazine ring amide silica gel stationary phase for liquid chromatograph and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The preparation method proceeds as follows:

[0030] a. Weigh the porous silica gel and immerse in the hydrochloric acid solution, disperse evenly by ultrasonic wave, reflux and stir at 110°C for 15h, filter, wash with water until neutral, then wash with absolute ethanol, and vacuum dry at 140°C for 12h; the silica gel and hydrochloric acid The dosage ratio of the solution is 1g: 20ml; the hydrochloric acid solution is a water dilution of concentrated HCl, and the volume ratio of concentrated HCl to water is 1:1; the porous silica gel has a particle size of 5 μm, a pore size of 120 ?, and a specific surface area of ​​290 m 2 / g;

[0031] b. Put the acidified silica gel into a three-necked flask, add toluene under the protection of nitrogen, stir and mix well, then slowly add γ-aminopropyltriethoxysilane, stir in an oil bath at 115°C for 17 h, and then use toluene, methanol, Dichloromethane was washed and suction filtered, and vacuum-dried at 60° C. for 12 h in a vacu...

Embodiment 2

[0036] The preparation method proceeds as follows:

[0037] a. Weigh the porous silica gel and immerse it in the hydrochloric acid solution, disperse it evenly by ultrasonic wave, stir it under reflux at 110°C for 18 h, filter it, wash it with water until neutral, then wash it with absolute ethanol, and dry it under vacuum at 140°C for 12 h; the silica gel and The dosage ratio of hydrochloric acid solution is 1g: 20ml; the hydrochloric acid solution is a water dilution of concentrated HCl, and the volume ratio of concentrated HCl to water is 1:1; the porous silica gel has a particle size of 5 μm, a pore size of 120 ?, and a specific surface area of ​​290 m 2 / g;

[0038] b. Put the acidified silica gel into a three-necked flask, add toluene under the protection of nitrogen, stir and mix well, then slowly add γ-aminopropyltriethoxysilane, stir in an oil bath at 110°C for 24 hours, and then use toluene, methanol, Wash and filter with methyl chloride, and vacuum dry at 60°C fo...

Embodiment 3

[0043] The preparation method proceeds as follows:

[0044] a. Weigh the porous silica gel and immerse it in the hydrochloric acid solution, disperse it evenly by ultrasonic wave, stir it under reflux at 110°C for 12 h, filter it, wash it with water until neutral, then wash it with absolute ethanol, and dry it in vacuum at 140°C for 12 h; the silica gel and The dosage ratio of the hydrochloric acid solution is 1g:20ml; the hydrochloric acid solution is a water dilution of concentrated HCl, and the volume ratio of concentrated HCl to water is 1:1; the porous silica gel has a particle size of 1.8 μm, a pore size of 100 ?, and a specific surface area 390m 2 / g;

[0045] b. Put the acidified silica gel into a three-necked flask, add toluene under the protection of nitrogen, stir and mix well, then slowly add γ-aminopropyltriethoxysilane, stir in an oil bath at 120°C for 12 h, and then use toluene, methanol, Dichloromethane was washed and suction filtered, and vacuum-dried at 6...

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Abstract

The invention discloses an embedded triazine ring amide silica gel stationary phase for liquid chromatograph and a preparation method thereof, wherein the embedded triazine ring amide silica gel stationary phase has high bonding quantity and stable bonding layer and contains two polar functional groups of triazine ring and amide. The structural formula of the obtained stationary phase is shown in the specification.

Description

technical field [0001] The invention relates to a stationary phase of liquid chromatography, especially a kind of silica gel embedded with triazine ring amide for liquid chromatography with high bonding amount, stable bonding layer, and two polar functional groups of triazine ring and amide Stationary phase and preparation method. Background technique [0002] High-performance liquid chromatography is currently the fastest-growing and most widely used analysis and separation technology. It is characterized by high sensitivity, high selectivity, high column efficiency, good repeatability, and easy operation. It is widely used in chemistry, medicine, food, environmental protection, and biochemistry. And industrial preparation and many other fields are playing an increasingly important role. The core of chromatographic separation is the chromatographic column, and the packing of the chromatographic column is the most critical part. Octadecyl bonded silica gel (ODS) has become...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30
Inventor 李萍沈从华唐涛孙元社王风云雷武李彤
Owner DALIAN ELITE ANALYTICAL INSTR
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