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Tetradocosyl heterocycle bonded silica gel chromatographic support, and preparation method and application thereof

A technology of docosyl and chromatographic stationary phase, which is applied in the field of tetraazadocosyl heterocyclic bonded silica gel chromatographic stationary phase and its preparation, and can solve the problems of single target analyte and limited stability. Achieve high separation efficiency, resistance to organic solvents, and wide application

Inactive Publication Date: 2017-12-19
GANSU AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problem that the imidazole ionic liquid functionalized high performance liquid chromatography stationary phase prepared by the prior art has limited stability and single target analyte in the detection of pesticide residues, the embodiment of the present invention provides a four Nitrodocosyl heterocyclic bonded silica gel chromatography stationary phase and its preparation method and application

Method used

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  • Tetradocosyl heterocycle bonded silica gel chromatographic support, and preparation method and application thereof
  • Tetradocosyl heterocycle bonded silica gel chromatographic support, and preparation method and application thereof
  • Tetradocosyl heterocycle bonded silica gel chromatographic support, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Example 1 Preparation of Sil-4N-22R Tetraazadocosyl Heterocyclic Bonded Silica Gel Chromatographic Stationary Phase

[0037] Steps:

[0038] ① 3g of silica gel was heated to reflux with concentrated hydrochloric acid for 4 hours, washed with water until neutral, and dried in vacuum at 120°C for 6 hours to obtain surface-activated silica gel.

[0039] ② Dissolve 6 mmol of acrolein and equimolar hexamethylenediamine together in 50 ml of perchloric acid solution, stir well, and undergo a ring closure reaction to form a docoheterocyclic ligand.

[0040] ③ Weigh 6 mmol of dococyclic ligand and dissolve in 40 ml of tetrahydrofuran solution, mix with 20 ml of tetrahydrofuran solution of equimolar γ-isocyanopropyltriethoxysilane, place at room temperature, and let stand for 30 minutes. Then, stirred for 12h, heated to 70°C, and refluxed for 2h. Formation of the docoheterocyclosilane reagent.

[0041] 4. add 3g acidified silica gel in the third step gained docosylcyclosilane ...

Embodiment 2

[0043] Example 2 Preparation of Sil-4N-22R Tetraazadocosyl Heterocyclic Bonded Silica Gel Chromatographic Stationary Phase

[0044] Steps:

[0045] ① 2.5g of silica gel was heated to reflux with concentrated hydrochloric acid for 4 hours, washed with water until neutral, and dried in vacuum at 120°C for 6 hours to obtain surface-activated silica gel.

[0046]② Dissolve 5 mmol of acrolein and equimolar hexamethylenediamine in 40 ml of perchloric acid solution by weighing, and stir thoroughly to generate a ring-closing reaction to form a docoheterocyclic ligand.

[0047] ③ Weigh 5mmol of the dococyclic ligand and dissolve it in 30ml of tetrahydrofuran solution, mix with 15ml of tetrahydrofuran solution of equimolar γ-isocyanopropyltriethoxysilane, place it at room temperature, and let it stand for 20 minutes. Then, stirred for 10h, heated to 60°C, and refluxed for 1h. Formation of the docoheterocyclosilane reagent.

[0048] 4. add 2.5g acidified silica gel in the third step g...

Embodiment 3

[0050] Example 3 Preparation of Sil-4N-22R Tetraazadocosyl Heterocyclic Bonded Silica Gel Chromatographic Stationary Phase

[0051] Steps:

[0052] ①Heat 3.5g of silica gel with concentrated hydrochloric acid to reflux for 6 hours, wash with water until neutral, and dry in vacuum at 120°C for 8 hours to obtain surface-activated silica gel.

[0053] ② Dissolve 7 mmol of acrolein and equimolar hexamethylenediamine in 60 ml of perchloric acid solution by weighing, stir well, and a ring-closing reaction occurs to form a docoheterocyclic ligand.

[0054] ③ Weigh 7mmol of the docoheterocyclic ligand and dissolve it in 50ml of tetrahydrofuran solution, mix with 25ml of tetrahydrofuran solution of equimolar γ-isocyanopropyltriethoxysilane, place it at room temperature, and let it stand for 40 minutes. Then, stirred for 15h, heated to 80°C, and refluxed for 3h. Formation of the docoheterocyclosilane reagent.

[0055] 4. add 3.5g acidified silica gel in the third step gained docosahe...

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Abstract

The invention discloses a preparation method of a tetradocosyl heterocycle chromatographic support, and belongs to the field of preparation and application of high performance liquid chromatographic support. The method is operated according to the following steps: firstly performing acidizing on the surface of porous spherical silica gel for chromatography, washing the surface to neutral, realizing silica gel surface activation, then ensuring that acrolein and hexamethylenediamine are reacted through simple ring-closure reaction to produce docosyl heterocycle ligand to be reacted with gamma-isocyanatopropyltriethoxysilane, and ensuring that silane heterocycle formed through synthesis is modified to the surface of a silica gel carrier, so as to obtain a tetradocosyl heterocycle bonded silica gel chromatographic support (Sil-4N-22R) with excellent separation and selection properties. High efficiency and high selectivity of a stationary phase are realized.

Description

technical field [0001] The invention belongs to the field of silica gel chromatographic stationary phases, and in particular relates to a silica docosyl heterocyclic bonded silica gel chromatographic stationary phase and a preparation method and application thereof. Background technique [0002] Pesticide residues are harmful to human body and environment. Pesticide residues are divided into mineral, biological, chemical and hormone categories according to their sources. According to the purpose, there are insecticides, acaricides, fungicides, biological agents, and growth regulators. The variety and scope of the compounds involved have brought great difficulty to the detection and monitoring of pesticide residues. [0003] Nitrogen heterocyclic compounds (NHCs) are the most common class of heterocyclic long-chain compounds, containing at least one R-amino group. The earliest work on the synthesis of nitrogen heterocycles can be traced back to the 1960s. O’fele and Wanzli...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/30G01N30/02
CPCB01J20/286G01N30/02
Inventor 蒋琼郭鸿儒杨宝生王森山刘长仲
Owner GANSU AGRI UNIV
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