Fe3O4-COOH magnetic nano-material modified open tubular column as well as preparation method and application thereof

A magnetic nano, fe3o4-cooh technology, applied in the field of chromatography, to achieve the effect of inhibiting adsorption, good hydrophilic performance and electrostatic effect, and improving separation selectivity

Active Publication Date: 2015-09-23
SOUTH CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few reports on the application of magnetic nanomaterials in the field of separation science, especially in the separation of biological samples.

Method used

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  • Fe3O4-COOH magnetic nano-material modified open tubular column as well as preparation method and application thereof
  • Fe3O4-COOH magnetic nano-material modified open tubular column as well as preparation method and application thereof
  • Fe3O4-COOH magnetic nano-material modified open tubular column as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Example 1: PDDAFe 3 o 4 Preparation of -COOH MNPs open-tube column

[0046] (1) Fe 3 o 4 Preparation of -COOH MNPs: 6 mM FeCl 3 ·6H 2 O was added to 40mL of diethylene glycol for ultrasonic-assisted dissolution, then 55mM anhydrous sodium acetate and 48mM sodium acrylate were added, stirred in a constant temperature water bath at 70°C at a speed of 500r / min for 1h to form a homogeneous solution, and the solution was poured into a special Put it in a Teflon high-pressure reactor, put it in an oven, raise the temperature to 200°C, react for 10 hours, cool to room temperature, separate the product under an external magnetic field and wash it with de-ethanol and deionized water for 3 times, and dry at 50°C to obtain dispersion Uniform Fe 3 o 4 -COOH MNPs magnetic particles.

[0047] (2) Capillary pretreatment: wash 1mol / L HCl at a flow rate of 10 μL / min for 1 hour to remove organic matter on the inner surface of the capillary, deionized water for 1 hour to remove ex...

Embodiment 2

[0051] Example 2: PDDAFe 3 o 4 Preparation of -COOH MNPs open-tube column

[0052] (1) Fe 3 o 4 Preparation of -COOH MNPs: 8 mM FeCl 3 ·6H 2 O was added to 40mL of diethylene glycol for ultrasonic-assisted dissolution, then 50mM anhydrous sodium acetate and 40mM sodium acrylate were added, stirred in a constant temperature water bath at 50°C at a speed of 300r / min for 1h to form a uniform solution, and the solution was poured into a special Put it in a Teflon high-pressure reaction kettle, put it in an oven, raise the temperature to 180°C, react for 15 hours, cool to room temperature, separate the product under an external magnetic field and wash it with de-ethanol and deionized water for 3 times, and dry at 40°C to obtain the dispersion. Uniform Fe 3 o 4 -COOH MNPs magnetic particles.

[0053] (2) Capillary pretreatment: wash 1.5mol / L HCl at a flow rate of 15μL / min for 1.5h to remove organic substances on the inner surface of the capillary, deionized water for 1.5h to...

Embodiment 3

[0056] Example 3: PDDAFe 3 o 4 Preparation of -COOH MNPs open-tube column

[0057] (1) Fe 3 o 4 Preparation of -COOH MNPs: 10 mM FeCl 3 ·6H 2 O was added to 40mL of diethylene glycol for ultrasonic-assisted dissolution, then 60mM anhydrous sodium acetate and 50mM sodium acrylate were added, stirred in a constant temperature water bath at 60°C at a speed of 400r / min for 1h to form a uniform solution, and the solution was poured into a special Put it in a Teflon high-pressure reaction kettle, put it in an oven, heat up to 190°C, react for 20 hours, cool to room temperature, separate the product under an external magnetic field and wash it with de-ethanol and deionized water for 3 times, and dry at 50°C to obtain dispersion Uniform Fe 3 o 4 -COOH MNPs magnetic particles.

[0058] (2) Capillary pretreatment: Rinse 2mol / L HCl at a flow rate of 20 μL / min for 2 hours to remove organic substances on the inner surface of the capillary, deionized water for 2 hours to remove exce...

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Abstract

The invention belongs to the technical field of chromatography, and discloses an Fe3O4-COOH magnetic nano-material modified open tubular column as well as a preparation method and application thereof. The preparation method comprises the following steps: (1) preparing Fe3O4-COOH MNPs according to a hydrothermal method; (2) fixing PDDA on the inner wall of a capillary through electrostatic self-assembly; (3) adsorbing the Fe3O4-COOH MNPs to the surface of the PDDA through electrostatic self-assembly, so as to obtain the Fe3O4-COOH magnetic nano-material modified open tubular column. The Fe3O4-COOH magnetic nano-material modified open tubular column takes glycosylated magnetic particles as a chromatography stationary phase, has an excellent hydrophilic performance and electrostatic interaction due to rich carboxyl groups, and can be used for effectively inhibiting adsorption of a biological sample, performing excellent separation functions on acid protein, polypeptide, amino acid and the like, and effectively detecting the micro heterogeneity of glycosylated protein; the preparation method has the advantages that the conditions are mild, the operation is simple and convenient, and the repeatability and the reproducibility are high.

Description

technical field [0001] The invention belongs to the technical field of chromatography, in particular to a Fe 3 o 4 -COOH magnetic nanomaterial modified open-tubular column and its preparation method and application. Background technique [0002] The development of proteomics and biotechnology has put forward higher requirements for the analysis tools of biological samples. Electrochromatographic analysis combines the high selectivity of high performance liquid chromatography and the high efficiency of capillary electrophoresis, and has been widely used in the separation and analysis of many biological samples including amino acids, peptides and proteins. As one of the cores of capillary electrochromatography, different types of chromatographic columns have been developed, including monolithic columns, packed columns, and open-tubular columns. Among these different forms of chromatographic columns, open-tube columns are widely favored by people because of the advantages of...

Claims

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Application Information

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IPC IPC(8): G01N30/60
Inventor 贾丽王文涛
Owner SOUTH CHINA NORMAL UNIVERSITY
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