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Tetranitrodocosyl heterocyclic ring chromatographic stationary phase and preparation method and application thereof

A behenyl, chromatographic stationary phase technology, applied in the field of functional material synthesis, can solve the problems of single target analyte species, low degradation rate, and high requirements for separation conditions, and achieves simple chromatographic analysis conditions, simple and good preparation methods. The effect of the application foreground

Active Publication Date: 2016-06-15
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, although aniline pesticides have a relatively strong insecticidal effect, they are also highly toxic and harmful to the environment.
Its degradation rate is low or difficult to degrade in soil, which can cause destructive effects on the environment
[0006] At present, imidazole-based ionic liquid HPLC stationary phases are mostly used for the detection of pesticide residues. However, when imidazole-based ionic liquid-functionalized HPLC stationary phases are used to detect pesticide residues, the separation conditions are high, the stability is limited and the target single analyte

Method used

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  • Tetranitrodocosyl heterocyclic ring chromatographic stationary phase and preparation method and application thereof
  • Tetranitrodocosyl heterocyclic ring chromatographic stationary phase and preparation method and application thereof
  • Tetranitrodocosyl heterocyclic ring chromatographic stationary phase and preparation method and application thereof

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Effect test

Embodiment 1

[0034] Preparation of Tetraazadocosyl Heterocyclic Chromatographic Stationary Phase

[0035] 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.

[0036] 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.

[0037] 3) Weigh 6 mmol of docoheterocyclic ligand and dissolve it in 40 ml of tetrahydrofuran solution, mix with equimolar γ-isocyanatopropyltriethoxysilane in tetrahydrofuran (20 ml) solution, and let stand at room temperature for 30 minutes. Then, it was stirred for 12 hours, heated to 70°C, and refluxed for 2 hours to generate a docosane cyclosilane reagent.

[0038] 4) in N 2 Under ambient conditions, add 3 g of the acidified silica gel prepared in the first step to the docohet...

Embodiment 2

[0041] Preparation of Tetraazadocosyl Heterocyclic Chromatographic Stationary Phase

[0042] 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.

[0043] 2) Dissolve 5 mmol of acrolein and equimolar hexamethylenediamine together in 40 ml of perchloric acid solution, stir well, and undergo a ring closure reaction to form a docoheterocyclic ligand.

[0044] 3) Weigh 5 mmol of docoheterocyclic ligand and dissolve in 30 ml of tetrahydrofuran solution, mix with equimolar γ-isocyanatopropyltriethoxysilane in tetrahydrofuran (15 ml) solution, and let stand at room temperature for 20 minutes. Then, it was stirred for 10 h, heated to 60° C., and refluxed for 1 h to generate a dococyclic silane reagent.

[0045] 4) in N 2 Under ambient conditions, add 2.5 g of the acidified silica gel prepared in the first step to the docosylcyclosil...

Embodiment 3

[0048] Preparation of Tetraazadocosyl Heterocyclic Chromatographic Stationary Phase

[0049] 1) 3.5g of silica gel was heated to reflux with concentrated hydrochloric acid for 6 hours, washed with water until neutral, and dried in vacuum at 120°C for 8 hours to obtain surface-activated silica gel.

[0050] 2) Dissolve 7 mmol of acrolein and equimolar hexamethylenediamine together in 60 ml of perchloric acid solution, stir well, and undergo a ring closure reaction to form a docoheterocyclic ligand.

[0051] 3) Weigh 7mmol of the docoheterocyclic ligand and dissolve it in 50ml of tetrahydrofuran solution, mix with an equimolar solution of γ-isocyanatopropyltriethoxysilane in tetrahydrofuran (25ml), and let stand at room temperature for 40 minutes. Then, it was stirred for 15 hours, heated to 80°C, and refluxed for 3 hours to generate a dococyclic silane reagent.

[0052] 4) in N 2 Under ambient conditions, add 3.5 g of the acidified silica gel prepared in the first step to the...

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Abstract

The invention discloses a tetranitrodocosyl heterocyclic ring chromatographic stationary phase. A preparation method includes: using hydrochloric acid to acidize porous spherical silica gel for chromatography, and water washing to neutral to realizing activation of the surface of silica gel; utilizing closed ring reaction to enable docosyl heterocyclic ring ligand generated by reaction of acrylic aldehyde and hexamethyldiamine to react with gamma-isocyanatepropyltriethoxy silane, and modifying a synthetic silane heterocyclic ring on the surface of a silica gel carrier to realize high efficiency and high selectivity of the stationary phase. The tetranitrodocosyl heterocyclic ring chromatographic stationary phase prepared by the method has excellent physical structure of silica gel matrix and has special chromatographic performance of nitrogen containing micro-ring; a structure of multi-nitrogen multi-alkyl heterocyclic ring long chain is bonded on the surface of silica gel, so that the stationary phase has high hydrophobicity and has certain hydrophilicity, thereby having high separating performance on pesticide residue (polycyclic aromatic hydrocarbons, phenols and amine); chromatographic analysis conditions after optimization are simpler and more convenient and easy to operate, so that application prospect is quite good.

Description

technical field [0001] The invention relates to functional material synthesis technology, in particular to a tetraazadocosyl heterocyclic chromatographic stationary phase, and also relates to a preparation method and application of the stationary phase. Background technique [0002] Pesticide residues are harmful to human body and environment. In general, pesticide residues can be divided into minerals, biology, chemicals, and hormones according to their sources; they can be divided into insecticides, acaricides, fungicides, and biological growth regulators according to their uses; many types of compounds are involved , The wide range has brought great difficulties to the detection and monitoring of pesticide residues. [0003] Polycyclic aromatic hydrocarbons (PolycyclicAromaticHydrocarbonsPAHs) refer to the volatile hydrocarbons produced when organic substances such as organic polymers contained in pesticides are not completely degraded, and are an important class of envi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/288B01J20/30
CPCB01J20/288B01J2220/52
Inventor 蒋琼邱红灯杜慧芳袁雪生吴宁鹏张书胜
Owner ZHENGZHOU UNIV
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