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Sol-gel chitosan grafting cyclodextrin capillary electrochromatography open tubular column

A technology of capillary electrochromatography and chitosan, which is applied in the field of sol-gel chitosan grafted cyclodextrin capillary electrochromatography open-tube column and its preparation, and achieves good chromatographic performance, firm bonding and improved separation effect. Effect

Inactive Publication Date: 2014-09-10
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no relevant report on the use of chitosan grafted cyclodextrin for open-tubular columns

Method used

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  • Sol-gel chitosan grafting cyclodextrin capillary electrochromatography open tubular column
  • Sol-gel chitosan grafting cyclodextrin capillary electrochromatography open tubular column
  • Sol-gel chitosan grafting cyclodextrin capillary electrochromatography open tubular column

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Experimental program
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Effect test

Embodiment 1

[0022] Embodiment 1: Sol-gel method prepares chitosan grafted cyclodextrin capillary electrochromatography open-tube column preparation:

[0023] (1) Capillary silanization:

[0024] Add 10%-30% tetramethoxysilane solution in toluene (anhydrous) to a certain length of capillary tube that has been treated with HCl and NaOH respectively, inject the capillary tube, seal it, and heat it at 90°C for 1.5h. Wash with methanol for 30 minutes, pass nitrogen gas at 70°C for 3 hours, and blow dry.

[0025] (2) Preparation of sol-gel:

[0026] Take 1-5mg of chitosan-grafted cyclodextrin (synthetic reference: Journal of Beijing Institute of Technology, 2005, 25(4): 372-376) dissolved in 1mL 2% (v%) acetic acid solution, add 100-400 micro l Gamma-glycidyl etheroxypropyl trimethoxysilane, ultrasonication at 0-10°C for 1h.

[0027] (3) In-column modification:

[0028] The sol-gel prepared in (2) was injected into the silanized capillary column, sealed, and the temperature was programmed: ...

Embodiment 2

[0029] Example 2: The effect of the concentration of chitosan-grafted cyclodextrin on the electroosmotic flow of capillary electrochromatography open column.

[0030] The effect of the quality of chitosan-grafted cyclodextrin on electroosmotic flow was characterized by electroosmotic flow. figure 1 Characteristics of electroosmotic flow in open-tubular columns prepared for solutions of different chitosan-grafted cyclodextrin concentrations. Phosphate buffer (pH 2.6, 5mmol / L) was used as the mobile phase, the separation voltage was ±15kV, the detection wavelength was 214nm, and thiourea was used as the electroosmotic flow marker.

Embodiment 3

[0031] Example 3: The effect of the concentration of chitosan-grafted cyclodextrin on the separation of xanthate isomers by capillary electrochromatography open-tube column.

[0032] figure 2 Separation of xanthine isomers by open-tubular columns prepared for different chitosan-grafted cyclodextrin concentrations. The inner diameter of the open-tube column is 50 μm, the total length is 60.0 cm, and the effective length is 35.0 cm; phosphate buffer (pH 2.6, 5 mmol / L) is used as the mobile phase, the separation voltage is -15 kV, and the detection wavelength is 303 nm. The order of elution is: isoxantterin, xantterin.

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Abstract

The invention discloses a sol-gel chitosan grafting cyclodextrin capillary electrochromatography open tubular column as well as a preparation method and application thereof, which belongs to the field of a chromatographic technology. The preparation method of the sol-gel chitosan grafting cyclodextrin capillary electrochromatography open tubular column comprises the following steps: (1) capillary pretreatment; (2) capillary surface silanization; (3) sol-gel preparation; and (4) inner capillary wall decoration. A stationary phase of the capillary open tubular column is chitosan grafting cyclodextrin sol-gel. The sol-gel chitosan grafting cyclodextrin capillary electrochromatography open tubular column provided by the invention combines the identification property of cyclodextrin and the adsorption property of chitosan. An obtained coating has the characteristics of firmness in bonding, stable property and good repeatability, and can be used within a wider pH (Potential of Hydrogen) range; the direction and the size of electroosmotic flow of the coating can be controlled by adjusting a pH value of a mobile phase; and the obtained coating has a good separation effect on Xanthopterin isomers and phenoxy carboxylic acid herbicides.

Description

technical field [0001] The invention belongs to the technical field of capillary electrochromatography, and in particular relates to a sol-gel chitosan grafted cyclodextrin capillary electrochromatography open column, a preparation method and application thereof. Background technique [0002] Capillary electrochromatography (CEC) is an efficient and fast new chromatographic micro-separation technology developed in recent years. As an important part of electrochromatographic separation technology, CEC columns can be divided into open-tubular columns, packed columns and monolithic columns. Among them, the open-tube column does not need to prepare a plug, and has the characteristics of simple preparation, easy control, and high column efficiency. There are three main preparation methods for open-tubular columns: coated polymer stationary phase, bonded stationary phase after surface roughening, and sol-gel (Sol-gel) technology. Sol-gel technology is a combination of capillary ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/22B01J20/30B01J20/285G01N30/02C07D475/04C07C51/47C07C59/68
Inventor 吕海霞李青音谢增鸿
Owner FUZHOU UNIV
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