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Porous metal oxide-silica gel liquid chromatogram filling material, and preparation method thereof

A porous metal and liquid chromatography technology, which is applied in the field of metal oxide-silica gel microsphere packing and its preparation, can solve problems such as tailing, achieve the effects of small steric hindrance, solve peak tailing, and avoid strong adsorption

Active Publication Date: 2019-06-07
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, when metal oxide-silica gel microspheres are used as hydrophilic chromatographic fillers, it is difficult to inhibit the adsorption of analytes by adjusting the pH of the solution due to the residual Lewis acidic sites on the surface, resulting in the metal oxides prepared by the prior art Oxide-silica fillers cause severe tailing for some polar analytes (J.Chromatogr.A 1522(2017)30)

Method used

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  • Porous metal oxide-silica gel liquid chromatogram filling material, and preparation method thereof

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Embodiment 1

[0025] Example 1: The inner and outer surfaces of porous silica gel microspheres are modified with zirconia-titania hybrid materials to form a zirconia-titania-silica gel matrix. The method refers to the document (Chinese invention patent, 201510920926.7), wherein the mass fraction of zirconium About 2%, the mass fraction of titanium is about 2%, and the specific surface area of ​​the porous silica microsphere is 350m 2 / g, the particle size is 5μm, the pore size is 10nm; the specific surface area of ​​the zirconia-silica gel matrix is ​​300m 2 / g. D-glucose-6-phosphate groups are modified on the surface of zirconia-titania-silica gel matrix. The modification process is to configure 20ml of D-glucose-6-phosphate disodium aqueous solution with a concentration of 0.03mol / L, and weigh zirconia-6-phosphate Soak 0.2 g of silica gel microspheres in the above solution and stir for 12 hours at a water temperature of 60°C to obtain a surface-modified D-glucose-6-phosphate group zircon...

Embodiment 2

[0030]The inner and outer surfaces of porous silica gel microspheres are decorated with zirconia-titania hybrid materials to form a zirconia-titania-silica gel matrix. The method refers to the document (Chinese invention patent, 201510920926.7), wherein the mass fraction of zirconium is about 3%. , the mass fraction of titanium is about 5%, and the specific surface area of ​​the porous silica microsphere is 150m 2 / g, the particle size is 5μm, and the pore size is 10nm; the specific surface area of ​​the zirconia-silica gel matrix is ​​140m 2 / g. D-fructose-1,6-diphosphate groups are modified on the surface of zirconia-titania-silica gel matrix, and the modification process is to prepare 10ml of D-fructose-1,6-diphosphate trisodium aqueous solution with a concentration of 200mM, and weigh Disperse 0.4 g of zirconia-silica gel microspheres in the above solution and heat and stir for 10 hours at a water temperature of 55°C to obtain a zirconia-silica gel material with surface-m...

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Abstract

The invention discloses a porous metal oxide-silica gel liquid chromatogram filling material, and a preparation method thereof. According to the preparation method, the surface of a zirconia-silica gel, titanium oxide-zirconia-silica gel, or titanium oxide-silica gel matrix is modified with D-glucose-6-phosphate groups or D-fructose-1, 6-diphosphate groups, and fosfomycin sodium is adopted for endcapping processing. Compared with conventional adenosine monophosphate group or fructose bisphosphate group modified zirconia-silica gel chromatogram filling materials, the advantages are that: at hydrophilic effect mode, the porous metal oxide-silica gel liquid chromatogram filling material possesses better chromatogram separation performance; compared with conventional silica gel surface saccharide group modification method, the preparation method is simpler, and is friendly to the environment; the silica gel microspheres modified with metal oxides such as zirconia and titanium oxide can beused steadily at a pH value range of 1 to 14; and the application prospect is promising.

Description

technical field [0001] The invention relates to the field of liquid chromatography, in particular to a metal oxide-silica gel microsphere filler for hydrophilic chromatographic separation and a preparation method thereof. Background technique [0002] Metal oxide-silica gel microspheres have good thermal stability and chemical stability, and this type of material is widely used in chromatographic separation and sample pretreatment (J.Chromatogr.A, 1028 (2004) 1; Anal.Chem., 86 (2014) 10122). The surface of metal oxide-silica gel microspheres has abundant Lewis acidic sites. In order to carry out chromatographic separation better, someone invented adenosine monophosphate-modified zirconia-silica gel liquid chromatography filler (J.Chromatogr.A 1383(2015 )58) and bisphosphofructose-modified zirconia-silica gel liquid chromatography filler (J.Chromatogr.A 1522(2017)30), and use it for hydrophilic chromatographic separation. [0003] Currently, LC packings used in the separati...

Claims

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Application Information

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IPC IPC(8): B01J20/283B01J20/30B01D15/30G01N30/02
Inventor 宋志花段春凤关亚风
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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