Histidine-modified organic-silica hybrid monolithic column, preparation method and application of monolithic column

A technology of silica gel hybridization and histidine, which is applied in the field of chromatographic packing, can solve the problems of complicated preparation method, uneconomical, poor separation of polar compounds, etc., and achieves a simple preparation method, solves inherent defects, and has a green preparation method. Effect

Active Publication Date: 2017-10-27
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In view of the above-mentioned prior art, in order to solve the complex, uneconomical, unenvironmental and other problems of the preparation method of the prior art, and at the same time solve the problem that the existing monolithic column material cannot achieve good separation of polar compounds, the present invention provides a composition Amino acid-modified organic silica-hybrid monolithic column, and provided its preparation method, and applied it to realize the separation and analysis of some common polar compounds and hydrophilic compounds

Method used

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  • Histidine-modified organic-silica hybrid monolithic column, preparation method and application of monolithic column
  • Histidine-modified organic-silica hybrid monolithic column, preparation method and application of monolithic column
  • Histidine-modified organic-silica hybrid monolithic column, preparation method and application of monolithic column

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Example 1 Preparation and application of histidine-modified organosilica-hybrid monolithic column

[0040] Proceed as follows:

[0041] ①Pretreatment of the capillary: Take a fused silica capillary with a length of 45 cm, wash it with methanol and water for 20 min, and then wash it with 1 mol / L NaOH solution, water, and 1 mol / L hydrochloric acid for 2.0 h, respectively. 0.5 h, 1.5 h, and then rinse the capillary with water for 20 min until the pH of the flushed liquid is neutral, and finally rinse with methanol for 20 min, and dry it with nitrogen at 120 °C for use;

[0042] ② Dissolve 240 mg polyethylene glycol (PEG, M=10 000) in a glass bottle filled with 2.5 mL 0.01 M acetic acid aqueous solution, and then slowly add 0.9 mL tetramethoxysilane (TMOS) and 0.3 mL Chloropropyltrimethoxysilane (CPTMS), the mixed solution was reacted for 4 h under ice-water bath conditions until a uniform and transparent sol was formed, and then the sol was ultrasonicated for 3 min under ...

Embodiment 2

[0045] Example 2 Preparation and application of histidine-modified organic-silica hybrid monolithic column

[0046] Proceed as follows:

[0047] ①Pretreatment of the capillary: Take a fused silica capillary with a length of 40 cm, wash it with methanol and water for 20 min, and then wash it with 1 mol / L NaOH solution, water, and 1 mol / L hydrochloric acid for 2.0 h, respectively. 0.5 h, 1.5 h, and then rinse the capillary with water for 20 min until the pH of the flushed liquid is neutral, and finally rinse with methanol for 20 min, and dry it with nitrogen at 120 °C for use;

[0048] ② Dissolve 240 mg polyethylene glycol (PEG, M=10 000) in a glass bottle filled with 2.5 mL 0.01 M acetic acid aqueous solution, and then slowly add 0.9 mL tetramethoxysilane (TMOS) and 0.3 mL Chloropropyltrimethoxysilane (CPTMS), the mixed solution was reacted for 4 h under ice-water bath conditions until a uniform and transparent sol was formed, and then the sol was ultrasonicated for 3 min unde...

Embodiment 3

[0051] Example 3 Preparation and application of histidine-modified organic-silica hybrid monolithic column

[0052] Proceed as follows:

[0053] ①Pretreatment of the capillary: Take a fused silica capillary with a length of 50 cm, wash it with methanol and water for 20 min, and then wash it with 1 mol / L NaOH solution, water, and 1 mol / L hydrochloric acid for 2.0 h, respectively. 0.5 h, 1.5 h, and then rinse the capillary with water for 20 min until the pH of the flushed liquid is neutral, and finally rinse with methanol for 20 min, and dry it with nitrogen at 120 °C for use;

[0054] ② Dissolve 240 mg polyethylene glycol (PEG, M=10 000) in a glass bottle filled with 2.5 mL 0.01 M acetic acid aqueous solution, and then slowly add 0.9 mL tetramethoxysilane (TMOS) and 0.3 mL Chloropropyltrimethoxysilane (CPTMS), the mixed solution was reacted for 4 h under ice-water bath conditions until a uniform and transparent sol was formed, and then the sol was ultrasonicated for 3 min unde...

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Abstract

The invention discloses a histidine-modified organic-silica hybrid monolithic column, which can be used for segregation analysis of polar compounds in a water-rich chromatographic mode. The preparation method of the histidine-modified organic-silica hybrid monolithic column comprises: introducing a mixed solution of tetramethoxysilane and chloropropyltrimethoxysilane with a proper ratio into a pretreated capillary tube; performing heating and reacting to prepare a chloropropyl-silica hybrid monolithic column bed; flushing excessive histidine aqueous solution into the chloropropyl-silica hybrid monolithic column bed; and performing heating to obtain the histidine-modified organic-silica hybrid monolithic column. According to the invention, a polar monolithic column stationary phase is prepared by bonding water-soluble organic functional monomers, and the monolithic column can realize segregation analysis of a plurality of common polar and hydrophilic compounds (amide compounds, nucleoside and nucleoside basic groups, amino acids and benzoic acid derivatives) in a water-rich chromatographic mode.

Description

technical field [0001] The invention relates to a histidine-modified organic-silica gel hybrid monolithic column, a preparation method and application thereof, and belongs to the technical field of chromatographic packing. Background technique [0002] At present, most of the applications of monolithic column materials are mainly concentrated in reversed-phase chromatographic separation, represented by C18 columns. However, the problem with this type of monolithic column material is that it is difficult to achieve effective separation of polar compounds. In addition, in the preparation, the existing preparation methods generally use water-insoluble organic functional monomers as modifiers, which requires a large amount of organic solvents to be used in the preparation process, and the preparation method is relatively complicated, uneconomical and environmentally friendly. . Contents of the invention [0003] In view of the above-mentioned prior art, in order to solve the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/30B01J20/22B01J20/28B01J20/30
CPCB01D15/305B01J20/103B01J20/22B01J20/2805
Inventor 曹绪龙宋新旺刘煜潘斌林祝仰文郭兰磊石静王红艳严兰于群王丽娟李青华李彬陈晓彦李宗阳
Owner CHINA PETROLEUM & CHEM CORP
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