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
  • Application Information

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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 th

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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