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Silica gel chromatography filler and preparation method thereof

A silica gel chromatography, silica gel technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of poor retention of polar compounds, unstable peak area, poor separation selectivity, etc., to achieve increased polar range and good stability , the effect of simple method

Active Publication Date: 2021-12-28
月旭科技(上海)股份有限公司 +2
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0007] The purpose of the present invention is to provide a silica gel chromatographic filler and its preparation method to solve the problems of poor retention of polar compounds and poor separation selectivity of traditional reversed-phase chromatographic fillers, as well as the unsatisfactory peak shape of the target object under the HILIC chromatographic mode and the short retention time. A series of problems such as instability, unstable peak area and large baseline noise

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  • Silica gel chromatography filler and preparation method thereof
  • Silica gel chromatography filler and preparation method thereof
  • Silica gel chromatography filler and preparation method thereof

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preparation example Construction

[0042] The present invention also provides the preparation method of above-mentioned silica gel chromatographic filler, comprises the steps:

[0043] S1: Activate and pretreat the silica gel to obtain activated silica gel with silanol groups on the surface;

[0044] S2: Perform hydration treatment, that is, place the activated silica gel in water and stir to obtain hydrated silica gel; the water is preferably ultrapure water.

[0045] S3: Mix the hydrated silica gel, stereosilane coupling agent and other silane coupling agents in an organic solvent, and carry out stirring and reflux reaction to obtain the silica gel chromatography filler.

[0046] Specifically, the silica gel is preferably fully porous spherical silica gel, more preferably ultra-high purity fully porous spherical silica gel for chromatography. The particle size of the raw silica gel used for activation is preferably 3-10 μm, and the pore size is preferably The specific surface area is preferably 180-400m 2...

Embodiment 1

[0055] (1) Add 100 g of silica gel (5 μm, purchased from DAISO, Japan) into a 2 L glass reaction vessel, add 1000 mL of distilled water, stir for 30 minutes, filter, and repeat this step twice. Then add 1000mL of hydrofluoric acid aqueous solution with a mass ratio of 0.08%, stir for 24 hours, wash with distilled water until neutral, finally add 1000mL of acetone to wash, filter, and dry at 110°C for 12 hours to obtain activated silica gel;

[0056] (2) Weigh 100 g (5 μm, Specific surface area: 300m 2 / g), placed in a 2L glass material reaction vessel; 5g of ultrapure water was added to the reaction vessel, and stirred at 170 rpm for more than 30 minutes to obtain hydrated silica gel;

[0057] (3) Add the hydrated silica gel prepared in step (2) to the glass material reaction vessel, and add 800mL of dry anhydrous toluene solvent, stir at 170 rpm and add 44.08g bicyclo[2.2.1]hexyl - A mixture of two silane reagents, ethyltrichlorosilane and 6.87g chloromethyldimethylchloros...

Embodiment 2

[0060] (1) Add 100 g of silica gel (5 μm, purchased from DAISO, Japan) into a 2 L glass reaction vessel, add 1000 mL of distilled water, stir for 30 minutes, filter, and repeat this step twice. Then add 900mL of hydrofluoric acid aqueous solution with a mass ratio of 0.06%, stir for 24 hours, wash with distilled water until neutral, finally add 1000mL of acetone to wash, filter, and dry at 110°C for 12 hours to obtain activated silica gel;

[0061] (2) Weigh 100g of activated silica gel (5μm, Specific surface area: 300m 2 / g), placed in a 2L reaction vessel; 8g of ultrapure water was added to the glass reaction vessel, and stirred at 250 rpm for 30 minutes to obtain hydrated silica gel;

[0062] (3) Add the hydrated silica gel prepared in step (2) to the glass material reaction vessel, and add 800mL of dry anhydrous toluene solvent, stir at 170 rpm and add 44.08g bicyclo[2.2.1]hexyl - A mixture of two silane reagents, ethyltrichlorosilane and 8.52g chloroethylmethyldichloros...

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Abstract

The invention provides a silica gel chromatographic filler, comprising: silica gel and an organosilane coupling agent bonded on the surface of the silica gel, the organosilane coupling agent includes a stereosilane coupling agent and other silane coupling agents. The silica gel chromatographic packing provided by the present invention introduces a three-dimensional structure group with a steric hindrance effect to maintain hydrophobicity while increasing the polarity of the packing surface, so that the polar range of the analyzable compound is greatly improved; in addition , while improving the polarity, a certain degree of hydrophobicity is also taken into account, so that complex components can also be well retained and separated in the silica gel chromatographic filler of the present invention. The preparation method of the silica gel chromatographic filler of the present invention has the advantages of simple method, good stability, good reproducibility, etc., and is applicable to large-scale production.

Description

technical field [0001] The invention relates to a liquid chromatography filling material, in particular to a silica gel chromatography filling material and a preparation method thereof. Background technique [0002] High performance liquid chromatography (HPLC) is one of the fastest-growing separation techniques in the field of analytical chemistry since the 1970s. After decades of development and improvement, it has now become a It is an indispensable means in the fields of food, sanitation, and environmental protection testing. Chromatographic column is undoubtedly the core of the whole HPLC system. In the past 40 years, the development of HPLC is mainly attributed to two aspects of chromatographic instruments and chromatographic column packing technology. The research and development of various chromatographic packing materials is the basis for the wide application of HPLC methods. At present, reversed-phase liquid chromatography (RPLC) is the most widely used chromatog...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01J20/30
CPCB01J20/286B01J20/30
Inventor 薛昆鹏屠炳芳任兴发陈再洁李崟杨慧李良翔赵圣
Owner 月旭科技(上海)股份有限公司
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