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Preparation method of gold nanoparticle modification based open tubular column

A gold nanoparticle and open-tubular column technology, which is applied to measuring devices, instruments, scientific instruments, etc., to achieve good reproducibility, improve the effect of small open-tubular columns and strong bonding

Inactive Publication Date: 2013-10-02
FUZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Through a large number of literature surveys, at present, there is no report on open-tube capillary columns derivatized with dodecanethiolated gold nanoparticles bonded with 3-mercaptopropyl-trimethoxysilane

Method used

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  • Preparation method of gold nanoparticle modification based open tubular column
  • Preparation method of gold nanoparticle modification based open tubular column
  • Preparation method of gold nanoparticle modification based open tubular column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Preparation of open-tube column for capillary electrochromatography with gold nanoparticles bonded to dodecyl mercaptan:

[0024] (1) Synthesis of gold nanoparticles (reference: Southeast University Journal, 2003, 33(4): 471-474.): Take 100mL of pure water and heat it to 100-120℃, and take 1-2% chlorine 1mL of gold acid aqueous solution, heat and stir for 15-20min, then quickly add 3mL of 1-2% sodium citrate aqueous solution, stir for 30-60min, cool to room temperature, and set aside;

[0025] (2) Pretreatment of capillary tube: 1) 1mol / L HCl rinse for 20-40min; 2) secondary water rinse for 20-40min; 3) 1mol / L NaOH rinse for 15-18h; 4) secondary water rinse for 20-40min; 5) 0.1mol / L HCl rinse for 20-40min; 6) secondary water rinse for 20-40min; 7) acetone rinse for 20-40min; 8) 180℃ N 2 Next, blow dry for 3h.

[0026] (3) Silanization of the capillary: Take a pretreated capillary of appropriate length, inject 10-20vol% tetramethoxysilane in anhydrous toluene solution, and rea...

Embodiment 2

[0029] The transmission electron microscope of the open column of capillary electrochromatography with gold nanoparticles bonded to dodecyl mercaptan is shown as figure 1 Shown.

Embodiment 3

[0031] The electroosmotic flow characteristics of a capillary electrochromatographic open-tube column with gold nanoparticles bonded to dodecyl mercaptan under different pH conditions.

[0032] The electroosmotic flow characteristics of open-tube capillary electrochromatographic columns with gold nanoparticles bonded to dodecyl mercaptan under different pH conditions are as follows figure 2 Shown. The capillary inner diameter of the open column is 50μm, the capillary column length is 60cm (effective length 35cm), phosphate buffer (pH 3.0, 5mmol / L) is the mobile phase, the separation voltage is +15kV, the detection wavelength is 214nm, and thiourea is the electroosmotic flow marker Things.

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Abstract

The invention discloses a gold nanoparticle modification based open tubular column, and a preparation method and application thereof, and belongs to the technical field of chromatography. The preparation method comprises the following steps: (1) synthesis of a gold nanoparticle solution by a chemical reduction method; (2) pretreatment on the capillary; (3) silanization of the capillary; and (4) modification on inner wall of capillary. The preparation method provided by the invention employs 3-mercapto propyl-trimethoxy silane as a silanization reagent, so that the gold nanoparticles and mercapto groups are modified on the inner surface of the quartz column by chemical bonding; then lauryl mercaptan is added, and the mercapto group in the lauryl mercaptan can react with gold nanoparticles as well, thereby bonding on the inner wall of the capillary. The invention uses gold nanoparticles easily characteristics and SH groups covalently bonded, gold nanoparticles were prepared by modified open tubular capillary column. The invention utilizes the characteristic of gold nanoparticles of easy covalent bonding with -SH groups to prepare the gold nanoparticle modified open tubular column. The technology of using gold nanoparticles as a stationary phase of the open tubular capillary column improves the disadvantages of low volume and small phase ratio of the open tubular capillary column.

Description

Technical field [0001] The invention belongs to the technical field of capillary chromatographic columns, and in particular relates to a modified open-tube column based on gold nanoparticles and a preparation method and application thereof. Background technique [0002] Capillary electrochromatography is an efficient and fast new microcolumn separation method developed on the basis of the development of electrophoresis technology and high performance liquid chromatography in recent years. It fills the capillary column with a liquid chromatography stationary phase or bonds a stationary phase to the column wall, and drives the mobile phase with electroosmotic flow. The solutes are separated according to their distribution between the stationary phase and the mobile phase and their electrophoretic mobility. An electrical separation mode. The flow pattern of the mobile phase in capillary electrochromatography is the same as that of capillary electrophoresis. It is a flat flow patter...

Claims

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Application Information

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IPC IPC(8): G01N30/60
Inventor 吕海霞秦文菲易姣姣谢增鸿
Owner FUZHOU UNIVERSITY
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