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fe 3 o 4 ‑cooh magnetic nanomaterial modified open-tubular column and its preparation method and application

A magnetic nanometer and open-column technology is applied in the field of chromatography to achieve the effects of simple preparation method conditions, improved separation effect and good separation effect.

Active Publication Date: 2017-03-22
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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  • fe <sub>3</sub> o <sub>4</sub> ‑cooh magnetic nanomaterial modified open-tubular column and its preparation method and application
  • fe <sub>3</sub> o <sub>4</sub> ‑cooh magnetic nanomaterial modified open-tubular column and its preparation method and application
  • fe <sub>3</sub> o <sub>4</sub> ‑cooh magnetic nanomaterial modified open-tubular column and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Example 1: PDDA@Fe 3 O 4 -COOH MNPs open-tube column preparation

[0046] (1)Fe 3 O 4 -COOH MNPs preparation: add 6mM 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, and stirred in a constant temperature water bath at 70℃ at 500r / min for 1h to form a homogeneous solution. Pour the solution into the special Put into an oven, heat up to 200℃, react for 10h, and cool to room temperature. Separate the product under an external magnetic field and wash it with ethanol and deionized water three times in sequence. Dry at 50℃ to obtain dispersion Uniform Fe 3 O 4 -COOH MNPs magnetic particles.

[0047] (2) Capillary pretreatment: 1mol / L HCl was flushed sequentially at a flow rate of 10μL / min for 1h to remove organic substances on the inner surface of the capillary, deionized water for 1h to remove excess HCl, 1mol / L NaOH for 1h to etch the inner surface of the capillary ...

Embodiment 2

[0051] Example 2: PDDA@Fe 3 O 4 -COOH MNPs open-tube column preparation

[0052] (1)Fe 3 O 4 -COOH MNPs preparation: add 8mM FeCl 3 ·6H 2 O was added to 40 mL of diethylene glycol for ultrasonic assisted dissolution, then 50 mM anhydrous sodium acetate and 40 mM sodium acrylate were added, and stirred in a constant temperature water bath at 50°C at 300 r / min for 1 hour to form a homogeneous solution. Pour the solution into the special Put into an oven, heat up to 180℃, react for 15h, and cool to room temperature. Separate the product under an external magnetic field and wash it with ethanol and deionized water three times in sequence. Dry at 40℃ to obtain dispersion Uniform Fe 3 O 4 -COOH MNPs magnetic particles.

[0053] (2) Capillary pretreatment: 1.5mol / L HCl was flushed sequentially 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 remove excess HCl, 1.5mol / L NaOH for 1.5h to etch the capillary T...

Embodiment 3

[0056] Example 3: PDDA@Fe 3 O 4 -COOH MNPs open-tube column preparation

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

[0058] (2) Capillary pretreatment: 2mol / L HCl was sequentially flushed at a flow rate of 20μL / min for 2h to remove organic substances on the inner surface of the capillary, deionized water for 2h to remove excess HCl, 2mol / L NaOH for 2h to etch the inner surface of the capilla...

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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, and particularly relates to a Fe 3 O 4 -COOH magnetic nano material modified open tube column and its preparation method and application. Background technique [0002] The development of proteomics and biotechnology fields puts forward higher requirements for the analysis tools of biological samples. Electrochromatographic analysis combines the high selectivity of high performance liquid chromatography with 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 technology, different types of chromatographic columns have been developed, including monolithic columns, packed columns and open-tube columns. Among these different types of chromatographic columns, open-tube columns are widely favored by people due to the adv...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/60
Inventor 贾丽王文涛
Owner SOUTH CHINA NORMAL UNIVERSITY
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