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

A technology of triazine cyclic amides and liquid chromatography, which is applied to chemical instruments and methods, and other chemical processes, can solve problems such as not showing good separation effects, and achieve novel structure, high bonding amount, good identification and The effect of separation performance

Active Publication Date: 2014-12-10
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 is carried out in sequence as follows:

[0030] a. Weigh the porous silica gel and immerse it in a hydrochloric acid solution, disperse it uniformly by ultrasonic, and stir at 110 °C for 15 h, filter, wash with water until neutral, then wash with absolute ethanol, and vacuum dry at 140 °C for 12 h; 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 diameter of 120 μm, and a specific surface area of ​​290 m 2 / g;

[0031] b. The acidified silica gel was placed in a three-necked flask, toluene was added under the protection of nitrogen, γ-aminopropyltriethoxysilane was slowly added after stirring and mixed uniformly, and 115 °C oil bath was electromagnetically stirred for 17 h, and then toluene, methanol, Dichloromethane was washed...

Embodiment 2

[0036] The preparation method is carried out in sequence as follows:

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

[0038] b. The acidified silica gel was placed in a three-necked flask, toluene was added under nitrogen protection, γ-aminopropyltriethoxysilane was slowly added after stirring and mixed uniformly, and 110 °C oil bath was electromagnetically stirred for 24 h, and then toluene, methanol, and diethyl ether wer...

Embodiment 3

[0043] The preparation method is carried out in sequence as follows:

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

[0045] b. The acidified silica gel was placed in a three-necked flask, toluene was added under the protection of nitrogen, γ-aminopropyltriethoxysilane was slowly added after stirring and mixed uniformly, and 120 °C oil bath was electromagnetically stirred for 12 h, followed by toluene, methanol, Dichloromethan...

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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 liquid chromatography stationary phase, in particular to an embedded triazine ring amide silica gel for liquid chromatography which has high bonding amount and stable bonding layer and simultaneously contains two polar functional groups, a triazine ring and an amide. Stationary phase and preparation method. Background technique [0002] High performance liquid chromatography is currently the fastest growing and most widely used analytical separation technology. It has the characteristics of high sensitivity, high selectivity, high column efficiency, good repeatability and easy operation. It is widely used in chemistry, medicine, food, environmental protection, biochemical and industrial preparation and many other fields play 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...

Claims

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Application Information

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Patent Type & Authority Patents(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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