Tetraoxacalix[2]arene[2]triazine bonded silica stationary phase and preparation method and application thereof

A technology of bonding silica gel and oxygen cups, which is applied in the field of separation, can solve the problems of complex separation system and inability to meet the requirements of separation analysis, and achieve the effects of low preparation cost, stable bonding layer and high bonding capacity

Inactive Publication Date: 2011-06-29
ZHENGZHOU UNIV
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Problems solved by technology

Separation systems are becoming more and more complex, especially the analysis of actual samples puts forward higher requirements for chromatographic techniques, especially chromatographic stationary phases. At present, there are many kin...

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  • Tetraoxacalix[2]arene[2]triazine bonded silica stationary phase and preparation method and application thereof
  • Tetraoxacalix[2]arene[2]triazine bonded silica stationary phase and preparation method and application thereof
  • Tetraoxacalix[2]arene[2]triazine bonded silica stationary phase and preparation method and application thereof

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Embodiment Construction

[0019] The structural formula of the tetraoxacix [2] arene [2] triazine bonded silica gel stationary phase of the present invention is as follows figure 1 shown.

[0020] Its specific preparation method is:

[0021] 1. Activation of silica gel: Weigh a certain amount of porous silica gel and immerse in HCl / H 2 In O(1:3, v / v), the ratio of silica gel weight (g) to hydrochloric acid volume (ml) is 1:15-1:20. Soak for 12 h, reflux for 24-36 h under magnetic stirring to remove metal ions, then filter with a G5 sand core funnel, rinse repeatedly with double distilled water until neutral, finally wash twice with acetone, and dry at 160 °C After 10 h to remove the surface solvent and water, the activated silica gel with evenly distributed hydroxyl groups on the surface was obtained, which was stored in a desiccator for later use.

[0022] 2. Preparation of precursor silica gel: 2 Introductory tube, condenser tube, CaCl 2 Add a certain amount of 3-aminopropyltriethoxysilane to ...

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Abstract

The invention discloses a tetraoxacalix[2]arene[2]triazine bonded silica stationary phase with large bonding quantity and a stable bonding layer. The concrete preparation method comprises the following steps: in the presence of anhydrous potassium carbonate, 3-aminopropyltriethoxysilane silica reacts with the tetraoxacalix[2]arene[2]triazine in N2 at the temperature of 30-90 DEG C to obtain the tetraoxacalix[2]arene[2]triazine bonded silica stationary phase. Experimental result indicates that the calixarene bonded stationary phase synthesized by the method has the characteristics of relatively large bonding quantity, stable bonding layer and the like; and the method is easy, the preparation cost is low, and the preparation method is widely applicable. The tetraoxacalix[2]arene[2]triazine bonded silica stationary phase not only has the traditional ODS (octadecylsilane bonded silica) reversed-phase chromatography performance, but also can provide sites for various actions such as complexing, hydrogen bonding, pi-pi interaction, space matching and the like. Therefore, the tetraoxacalix[2]arene[2]triazine bonded silica stationary phase can replace ODS to some degree, and provide possibility in separating substances difficult to separate at the same time.

Description

technical field [0001] The invention relates to separation technology, in particular to a tetraoxacalix[2]arene[2]triazine bonded silica gel stationary phase with high bonding amount and stable bonding layer; the present invention also relates to a preparation method of the stationary phase and apply. Background technique [0002] High performance liquid chromatography plays a pivotal role in modern separation analysis. It is widely used in various fields such as chemistry, medicine, life science and environmental science, and has become an indispensable research method. Separation systems are becoming more and more complex, especially the analysis of actual samples puts forward higher requirements for chromatographic techniques, especially chromatographic stationary phases. At present, there are many kinds of commercially available silica gel and modified silica gel, among which octadecyl bonded silica gel (ODS) as the representative reversed-phase chromatographic station...

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Application Information

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IPC IPC(8): B01J20/283B01J20/30B01D15/08
Inventor 张书胜赵文杰于阿娟梁松程远胡锴冶保献
Owner ZHENGZHOU UNIV
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