Neutral hydrophilically-interacted hybrid silicagel-based monolithic column

A hybrid silica gel, hydrophilic technology, applied in the field of analytical chemistry, can solve the problems of difficult to prepare neutral silica gel monolithic column, difficult to eliminate silanol groups, etc., to meet the requirements of continuous separation, high mechanical strength and uniform internal structure.

Active Publication Date: 2012-08-15
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The present invention is based on a one-step polymerization reaction initiated by free radicals, and applies cage-like polyhedral siloxane nanomaterials to the preparation of neutral hydrophilic interaction hybrid silica monolithic columns, which solves the difficulty of eliminating silicon hydroxyl groups in traditional silica gel substrates and the difficulty in preparing neutral silica gel The problem of the monolithic column, the polymerization reaction and the distribution ratio of each component of the non-charged hydrophilic interaction hybrid silica monolithic column were established

Method used

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  • Neutral hydrophilically-interacted hybrid silicagel-based monolithic column
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  • Neutral hydrophilically-interacted hybrid silicagel-based monolithic column

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Embodiment 1

[0024] Organic monomer: hydroxyethyl methacrylate, polycage siloxane crosslinking agent: methyl methacrylate based cage oligomeric silsesquioxane, initiator: azobisisobutyronitrile, mixed Porogen: the mass ratio of toluene-dodecanol is prepared according to the following data respectively:

[0025] Column A: polycage siloxane crosslinker 7.0%, organic monomer: 23%, dodecyl alcohol: 35.0%, toluene: 34.0%, initiator 1%.

[0026] Column B: polycage siloxane crosslinker 7.0%, organic monomer: 23%, dodecyl alcohol: 26.8%, toluene: 42.2%, initiator 1%.

[0027] Column C: polycage siloxane crosslinker 7.0%, organic monomer: 23%, dodecyl alcohol: 19.0%, toluene: 50.0%, initiator 1%.

[0028] Column D: polycage siloxane crosslinker 7.0%, organic monomer: 23%, dodecyl alcohol: 10.9%, toluene: 59.1%, initiator 1%.

[0029] Column E: polycage siloxane crosslinker 5.1%, organic monomer: 24.9%, dodecyl alcohol: 19.0%, toluene: 50.0%, initiator 1%.

[0030] Column F: polycage siloxane cro...

Embodiment 2

[0034] Apply the monolithic column C prepared above, use acetonitrile:triethylamine phosphate buffer (5mmol / L, pH6.5)=94:6 as the mobile phase, the separation voltage is minus 20 kV, the auxiliary pressure is 1.1MPa, and the pump flow rate is 0.1 Under the condition of mL / min, the neutral amide compounds can achieve baseline separation on the non-charged hydrophilic interaction hybrid silica gel electrochromatographic column, and the elution peaks are as follows: 1. N, N-dimethylformamide; 2. . N, N-Dimethacrylamide; 3. Acrylamide; 4. Acetamide; 5. Formamide; 6. Thiourea.

[0035]Apply the monolithic column C prepared above, use acetonitrile: triethylamine phosphate buffer (2mmol / L, pH 6.5) = 90:10 as the mobile phase, the separation voltage is minus 15 kV, the auxiliary pressure is 3.5MPa, and the pump flow rate is 0.1 mL Under the condition of 1 / min, basic nucleosides and basic polar compounds are effectively separated on the non-charged hydrophilic interaction hybrid silica...

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Abstract

The invention discloses a neutral hydrophilically-interacted hybrid silicagel-based monolithic column which is composed of an uncharged polar organic monomer, a poly-cage type siloxane crosslinking agent, a porogenic agent and an initiator, wherein the uncharged polar organic monomer is hydroxyethyl methacrylate, the poly-cage type siloxane crosslinking agent is methylmethacrylate-based cage-like oligomeric silsesquioxane, the porogenic agent is a mixture of toluene and lauryl alcohols, and the initiator is azodiisobutyronitrile. The polymeric stationary phase of the silicagel-based monolithic column disclosed by the invention is distributed uniformly, the silicagel-based monolithic column is good in permeability and high in mechanical strength, the surface of the stationary phase has no hydroxyl, and the strong electrostatic adsorption between a charged compound and a silicon hydroxyl is solved; and the silicagel-based monolithic column contains rich neutral polar groups, so that the silicagel-based monolithic column can adsorb mobile-phase neutral ions on the surfaces of the stationary phases and provide a certain zeta potential so as to generate a relatively stronger electroosmotic flow, therefore, the silicagel-based monolithic column has a typical hydrophilically-interacted chromatographic performance, and can meet the requirements for the continuous rapid separation of polar neutral and alkaline compound materials.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a neutral hydrophilic interaction hybrid silica gel monolithic column. Background technique [0002] Capillary electrochromatography (CEC) is a fast and efficient micro-separation technology developed in recent years. As the core of CEC technology application, capillary electrochromatography column has become a research hotspot in the field of modern micro-separation. Capillary monolithic columns have been widely used in CEC separation systems due to their advantages of simple preparation, uniform internal structure, flexible surface modification, good biocompatibility, and no need for sintered plungers. [0003] Neutral monolithic column is a kind of monolithic stationary phase with a new mode of action developed in recent years. It is characterized in that the surface of the stationary phase does not have groups that can dissociate to generate strong charges, whi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/60
Inventor 林旭聪王啸谢增鸿
Owner FUZHOU UNIV
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