HPLC (high-performance liquid chromatography) chromatographic column packing modification method

A chromatographic column packing and modification technology, which is applied in the field of modifying the surface of silica microspheres by using photosensitive polymer diazo resin, can solve the problems of complicated and time-consuming preparation methods, unfriendly environment, etc., and achieve good Separation effect, easy availability of raw materials, and low production cost

Active Publication Date: 2015-08-12
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] For this reason, the technical problem to be solved by the present invention lies in the complex, time-consuming and environmentally unfriendly preparation methods of the existing HPLC chromatographic column fillers, and then provides a novel modification method for the HPLC chromatographic column fillers, which utilizes photosensitive polymer weight As a surface modifier, the nitrogen resin converts the hydrogen bond between the diazo resin and the silicon hydroxyl group on the surface of the silica microsphere into a covalent bond through the photocrosslinking reaction, thereby introducing hydrophobic groups on the surface of the microsphere. The modified chromatographic column packing has good separation effect

Method used

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  • HPLC (high-performance liquid chromatography) chromatographic column packing modification method
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  • HPLC (high-performance liquid chromatography) chromatographic column packing modification method

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Embodiment 1

[0037] The modification method of the HPLC chromatographic column filler silica microsphere of the present embodiment, comprises the following steps:

[0038] S1. Activation treatment of silica microspheres:

[0039] Disperse 0.5 g of monodisperse silica microspheres with a particle size of 2.5 μm uniformly in a strong alkali sodium hydroxide with a concentration of 0.1 mol / L for 30 minutes, centrifuge and wash the silica microspheres to neutrality;

[0040] S2, modifying the silica microspheres after the activation treatment:

[0041] The activated silica microspheres were placed in an aqueous solution of diazo resin with a concentration of 4 mg / mL, and reacted with magnetic stirring at room temperature for 2 hours in a light-proof environment, and then centrifuged, and the product was washed 3 times with deionized water, The obtained product was treated overnight in a vacuum drying oven, and the dried silica microspheres were exposed to ultraviolet light for 15 minutes to o...

Embodiment 2

[0045] The modification method of the HPLC chromatographic column filler silica microsphere of the present embodiment, comprises the following steps:

[0046] S1. Activation treatment of silica microspheres:

[0047]Disperse 0.5 g of monodisperse silica microspheres with a particle size of 1 μm uniformly in a strong alkali potassium hydroxide solution with a concentration of 0.08 mol / L for 45 minutes, centrifuge and wash the silica microspheres to neutrality;

[0048] S2, modifying the silica microspheres after the activation treatment:

[0049] The activated silica microspheres were placed in an aqueous solution of diazo resin with a concentration of 3 mg / mL, and reacted with magnetic stirring at room temperature for 3 hours in a light-proof environment, and then the product was washed twice with deionized water after centrifugation. The obtained product was treated overnight in a vacuum drying oven, and the dried silica microspheres were exposed to ultraviolet light for 20 ...

Embodiment 3

[0052] The modification method of the HPLC chromatographic column filler silica microsphere of the present embodiment, comprises the following steps:

[0053] S1. Activation treatment of silica microspheres:

[0054] Disperse 0.5 g of monodisperse silica microspheres with a particle size of 5 μm uniformly in a strong hydrochloric acid solution with a concentration of 0.15 mol / L for 20 minutes, centrifuge and wash the silica microspheres to neutrality;

[0055] S2, modifying the silica microspheres after the activation treatment:

[0056] The activated silica microspheres were placed in an aqueous solution of diazo resin with a concentration of 5 mg / mL, and reacted with magnetic stirring at room temperature for 4 hours in a light-proof environment, and then centrifuged, and the product was washed 3 times with deionized water, The obtained product was placed in a vacuum drying oven for overnight treatment, and the dried silica microspheres were exposed to ultraviolet light for ...

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Abstract

The invention relates to a HPLC (high-performance liquid chromatography) chromatographic column packing modification method. The method includes: putting HPLC chromatographic column packing in diazonium resin solution, stirring for reaction for 2-4h at the room temperature in a dark environment, carrying out centrifugal separation, washing and drying products, and performing exposure treatment under ultraviolet light for 10-20min. By adoption of photosensitive macromolecular diazonium resin as surface modifier, hydrogen-bonding interaction between the diazonium resin and surface silanol groups of silicon dioxide microspheres is converted into covalent bonding interaction by means of photo-crosslinking reaction, and accordingly hydrophobic groups can be introduced to the surface of the microsphere, and the modified chromatographic column packing has excellent separation effects.

Description

technical field [0001] The invention relates to a method for modifying HPLC chromatographic column packing, in particular to a method for modifying the surface of silica microspheres by using a photosensitive polymer diazo resin. Background technique [0002] High performance liquid chromatography (HPLC) is one of the most widely used analysis and separation methods nowadays, and is widely used in various fields of scientific research and social production such as separation and detection of various mixtures, qualitative and quantitative analysis. As the core part of liquid chromatography, chromatographic column has been highly valued because of its decisive role in analysis and separation. Therefore, in the past few decades, the research of novel chromatographic column packing materials has been receiving high attention. [0003] As one of the most widely used inorganic liquid chromatography column packings, silica is favored for its characteristics of good chemical stabil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/281B01J20/30
Inventor 丛海林于冰田超
Owner QINGDAO UNIV
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