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Preparation method of organic-inorganic hybridized monolithic column

A monolithic column and inorganic technology, applied in the field of organic-inorganic hybrid monolithic column and its preparation, to achieve the effect of uniform mesopore diameter, easy column filling operation, and compact monolithic column structure

Active Publication Date: 2013-06-26
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the technology of using Pluronic F127 and dodecylamine as a porogen to synthesize a hybrid monolithic column has not been reported yet.

Method used

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  • Preparation method of organic-inorganic hybridized monolithic column
  • Preparation method of organic-inorganic hybridized monolithic column
  • Preparation method of organic-inorganic hybridized monolithic column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1: Preparation of organic-inorganic hybrid monolithic column

[0026] Firstly, the inner wall of the capillary with 75 μm and 100 μm inner diameter is pretreated. Rinse the capillary with 0.1mol / L hydrochloric acid for 4 hours, rinse with water until neutral, then rinse with 1mol / L NaOH for 2 hours, then rinse with water and methanol for 0.5 hours respectively, and then keep it at 120°C for 3 hours under nitrogen, until it drops to After room temperature, seal both ends of the capillary for use.

[0027] Add 30 mg of Pluronic F127, 350 μL of methanol, 20 μL of water, and 20 μL of hydrochloric acid (0.5 mol / L) into a 1.5 mL centrifuge tube, and ultrasonically dissolve it completely. Add another 180 µL tetraethoxysilane, 100 µL octyltriethoxysilane, and vortex for 3 min. Put into 60 ℃ water bath and hydrolyze for 4 hours. After hydrolysis, put into ice water and cool to 0°C, add 6 mg of dodecylamine, vortex for 1 minute, draw the solution with a syringe, filter...

Embodiment 2

[0033] Example 2: Adjusting the overall column morphology and column efficiency by adjusting the amount of porogen

[0034] The synthesis method of the monolithic column is the same as in Example 1, and the composition of the specific synthesis raw materials is shown in Table 1. The column A is an octyl hybrid monolithic column made of a traditional one-component porogen. Columns B-D are monolithic columns made of binary porogens with different ratios of porogens.

[0035] Table 1: Raw material ratio of four kinds of monolithic columns in embodiment two

[0036]

[0037] Figure 4The scanning electron micrographs of columns A-D show that after the addition of Pluronic F127, the morphology of the overall column changes from aggregated spherical to typical bicontinuous structure. And with the increase of the amount of Pluronic F127 added, the material through-hole size becomes smaller. Because the formation of monolithic materials is the result of the combined action of p...

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Abstract

The invention discloses an organic-inorganic hybridized monolithic column as well as a preparation method and an application thereof. The monolithic column comprises a silica gel framework and has a typical reversed phase chromatographic mechanism through introducing octyl. According to the monolithic column, tetraethoxysilane is served as an inorganic monomer, octyltriethoxysilane is served as an organic-inorganic hybridized monomer, a binary porogenic agent Pluronic F127 / lauryl amine is used for substituting for the conventional single porogenic agent-lauryl amine, methanol / water is served as a solvent, hydrochloric acid and lauryl amine are used as acid-base regulators, and the monolithic column is synthesized by adopting a double-step acid-base sol-gel method. The monolithic column obtained by the method is of an ideal double-pore structure, a preparation process is simple and easy to operate, and high column efficiency is obtained. Through utilizing the synthesizing method of the monolithic column, naphthalene is served as an analyte, and the height of the obtained column plate is reduced to 20-30 micrometers from 70-80 micrometers. The hybridized monolithic column can be used for the reversed phase chromatographic separation and enrichment of various hydrophobic substances.

Description

technical field [0001] The invention belongs to the field of liquid chromatography column materials, and in particular relates to an organic-inorganic hybrid monolithic column and its preparation method and application. Background technique [0002] Since its appearance, the monolithic column has attracted more and more attention due to its advantages of simple preparation, good permeability, high mass transfer efficiency and diversity of surface modification. Currently, it is mostly used in microliter / nanoliter liquid chromatography and microfluidic chips. Research. People have used different monomers and cross-linking agents to make monolithic materials with different functional groups, which have been successfully used in reversed-phase, hydrophilic, ion-exchange and other separation modes of chromatography. The application objects involve environmental samples, biological macromolecules, Omics research of complex samples, etc. [0003] The current monolithic columns ar...

Claims

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Application Information

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IPC IPC(8): B01D15/22B01J20/281B01J20/30G01N30/60
Inventor 许国旺单圆鸿石先哲李华
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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