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Silica gel chromatographic packing as well as preparation method and application thereof

A technology of silica gel chromatography and silica gel, which is applied in the field of high-performance liquid chromatography packing materials, can solve the problems of unstable peak area, large baseline noise, and low column efficiency, and achieve the effects of simple preparation method, stable peak area, and high column efficiency

Inactive Publication Date: 2018-06-19
浙江月旭材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to provide a silica gel chromatographic filler for separation and content determination of lactose and a preparation method thereof. The silica gel chromatographic filler can solve the problems of low column efficiency and large peak area when the traditional amino chromatography column is used for content determination of lactose. Problems such as stability and baseline noise, with good reproducibility and stability

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  • Silica gel chromatographic packing as well as preparation method and application thereof
  • Silica gel chromatographic packing as well as preparation method and application thereof
  • Silica gel chromatographic packing as well as preparation method and application thereof

Examples

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preparation example Construction

[0042] The present invention also provides a method for preparing the above silica gel chromatographic filler, which includes the following steps:

[0043] The silica gel is activated and pretreated to obtain activated silica gel with silanol on the surface;

[0044] The activated silica gel and the other silane are stirred and refluxed in an organic solvent, and the other silane is bonded to the surface of the activated silica gel to obtain a solution containing organic-inorganic hybrid silica gel; and

[0045] Aminopropyl silane is added to the solution for stirring and reflux reaction, and the aminopropyl silane is bonded to the surface of the organic-inorganic hybrid silica gel to obtain the silica gel chromatographic filler.

[0046] Specifically, the silica gel is preferably a fully porous spherical silica gel, and more preferably an ultra-high purity fully porous spherical silica gel for chromatography. The particle size of the raw material silica gel for activation is preferab...

Embodiment 1

[0056] Example 1 Preparation of silica gel chromatography packing

[0057] figure 1 It is a schematic diagram of the method for preparing silica gel chromatography packing in Example 1. The specific preparation method includes the following steps:

[0058] (1) Add 100 g of silica gel (5 μm, purchased from Japan DAISO) into a 2L glass material reaction vessel, and add 1000 mL of distilled water, stir for 30 minutes, and filter, and repeat this step twice. Then add 1000 mL of 0.08% hydrofluoric acid aqueous solution with a mass ratio of 0.08%, stir for 24 hours and wash with distilled water to neutrality, finally add 1000 mL of acetone to wash, filter, and dry at 110°C for 12 hours to obtain activated silica gel A;

[0059] (2) Add the activated silica gel A prepared in "Step (1)" into the glass reaction vessel, and add 800 mL of dry anhydrous toluene solvent, stir well at 170 rpm, and then add 50.0 g of 1,2-bis(三甲 (Oxysilyl) propane B, use an electric heating mantle to heat to 110°C...

Embodiment 2

[0063] Example 2 Preparation of silica gel chromatography packing

[0064] (1) Add 100 g of silica gel (5 μm, purchased from Japan DAISO) into a 2L glass material reaction vessel, and add 1000 mL of distilled water, stir for 30 minutes, and filter, and repeat this step twice. Then add 1000 mL of 0.08% hydrofluoric acid aqueous solution with a mass ratio of 0.08%, stir for 24 hours and wash with distilled water to neutrality, finally add 1000 mL of acetone to wash, filter, and dry at 110°C for 12 hours to obtain activated silica gel;

[0065] (2) Add the activated silica gel prepared in "Step (1)" to the glass reaction vessel, and add 800 mL of dry anhydrous toluene solvent, stir well at 170 rpm, and then add 50.0 g of 1,2-bis(formaldehyde) (Oxysilyl)butane, heated to 110°C with an electric heating mantle, stirred and refluxed for 24 hours to obtain a solution containing organic-inorganic hybrid silica gel, wherein the organic-inorganic hybrid silica gel still contains part of unrea...

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Abstract

The invention provides a silica gel chromatographic packing as well as a preparation method and application thereof. The silica gel chromatographic packing is prepared from silica gel and organosilanewhich is bound to the surface of the silica gel; and the organosilane is prepared from aminopropyl silane and other silanes, wherein the aminopropyl silane is introduced into alkyl groups with the space steric effect. For the silica gel chromatographic packing provided by the invention, by introducing an organic-inorganic hybrid structure and the alkyl groups with the space steric effect, the stability of the silica gel chromatographic packing is effectively improved, and the silica gel chromatographic packing can enable lactose to have very excellent peak pattern, relatively high column efficiency and stable peak area when being used for lactose separation. In addition, the preparation method of the silica gel chromatographic packing has the advantages of simpleness, good stability, goodreproducibility, easiness in scale production and the like.

Description

Technical field [0001] The invention relates to a high-performance liquid chromatography packing material, in particular to a silica gel chromatography packing, a preparation method and an application thereof. Background technique [0002] Lactose is a disaccharide consisting of a molecule of β-D-galactose and a molecule of α-D-glucose at the β-1,4-position to form a glycosidic bond. The molecular formula is C 12 H 22 O 11 , The relative molecular mass is 342.3. Lactose has two anomeric isomers: α-lactose and β-lactose, which can be converted into each other in aqueous solution. Alpha-lactose easily binds to a molecule of crystal water. As a pharmaceutical excipient, lactose is widely used in tablets, capsules, granules and freeze-dried products in the form of fillers or diluents. At present, there are methods on the market that use hydrogen-type sugar columns or calcium-type sugar columns to separate lactose and other carbohydrate targets. Although hydrogen-type sugar columns ...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/30B01D15/08G01N30/02C07H1/06C07H3/04
CPCB01D15/08B01J20/286B01J2220/52C07H1/06C07H3/04G01N30/482
Inventor 薛昆鹏屠炳芳姚立新李金瑞李良翔郭德勇李崟王韶青
Owner 浙江月旭材料科技有限公司
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