Novel preparation method of monolithic column stationary phase having gradient distribution

A gradient distribution and monolithic column technology, applied in the field of chromatographic stationary phase, can solve problems such as easy generation of bubbles, cumbersome operation, gradient elution obstruction, etc., and achieve high column efficiency and high stability

Inactive Publication Date: 2012-02-01
EAST CHINA UNIV OF SCI & TECH
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Problems solved by technology

However, in capillary electrochromatography, the difficulty lies in the cumbersome operation and easy gener

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  • Novel preparation method of monolithic column stationary phase having gradient distribution
  • Novel preparation method of monolithic column stationary phase having gradient distribution
  • Novel preparation method of monolithic column stationary phase having gradient distribution

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[0046] Example 1

[0047] Weigh 0.1200g of EDMA, 0.1800g of BMA, 0.2880g of n-propanol, 0.1620g of 1,4-butanediol, and 0.0023g of AIBN into a 1.5mL centrifuge tube. Blow with nitrogen until the hot initiator dissolves. Weigh 0.0025g of magnetic nanoparticles into a 1.5mL centrifuge tube, measure 250uL of the above-mentioned BMA matrix into the magnetic nanomaterial, vortex for 1min to mix evenly, and then sonicate for 1min to prevent the magnetic nanoparticles from agglomerating. Extract to 15cm in the capillary, stand vertically for 3 hours, put it in an oven at 60°C for 22 hours (keep standing vertically), rinse the reacted capillary column with methanol first, and then rinse with water to wash away unreacted The residue is then equilibrated with the mobile phase for a period of time.

[0048]The invention realizes the gradient separation directly using the stationary phase without adjusting the mobile phase, and is especially suitable for the separation of complex samples...

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Abstract

The invention relates to a novel preparation method of a monolithic column stationary phase having gradient distribution, comprising the following steps: 1, pretreating a chromatographic column, 2, carrying out a preparation method of the monolithic column stationary phase having gradient distribution; and 3, preparing the monolithic column stationary phase having gradient distribution by using aspecial magnetic nano material. In the step 3, according to the preparation method disclosed in the step 2, magnetic nanoparticle-doped matrix of the monolithic column is rushed into a pretreated stainless steel tube or capillary tube, a coil or permanent strong magnetism is used to control the magnetic field intensity axially, heating reaction is carried out to solidify the matrix of the monolithic column to allow the magnetic nanoparticles to be distributed gradedly in the monolithic skeleton, so that the monolithic column stationary phase having gradient distribution is obtained. Accordingto the invention, the adjustment of the mobile phase is realized, and the stationary phase is used for gradient separation, so that the invention is suitable for separation of a complex sample; and the system has high column efficiency, high selectivity, and good repeatability of separation, and the preparation is easy to operate.

Description

【Technical field】 [0001] The invention relates to the technical field of chromatographic stationary phases, in particular to a novel method for preparing monolithic column stationary phases with gradient distribution. 【Background technique】 [0002] Chromatographic separation and analysis has become one of the most powerful tools for the separation and analysis of complex components in analytical chemistry. With the development of separation science, the separation of complex systems such as biological samples and traditional Chinese medicines has become a research hotspot, and higher and higher requirements are put forward for the preparation of chromatographic stationary phases. Gradient elution in traditional high performance liquid chromatography is to program control the composition of mobile phase in one analysis period, such as the polarity of solvent, ionic strength and pH value, etc. complex samples. The use of gradient elution can shorten the analysis time, impro...

Claims

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Application Information

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IPC IPC(8): B01J20/281B01J20/30G01N30/60
Inventor 张凌怡万莉雷雯郑翌覃飒飒张维冰
Owner EAST CHINA UNIV OF SCI & TECH
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