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Raw material prescription of opposite phase anion exchange electric chromatograph integral column and preparation thereof

A monolithic column and electrochromatography technology, applied in the field of electrochromatography, can solve the problems of cumbersome and time-consuming steps, and achieve the effect of simple process, good column permeability and less time

Inactive Publication Date: 2011-04-06
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Horváth et al. synthesized poly(glycidyl methacrylate-ethylene glycol dimethacrylate) and poly(chlorostyrene-divinylbenzene) in situ in a capillary, and then performed derivatization on the column to obtain Positively charged capillary electrochromatographic monolithic column, but the steps are slightly cumbersome and time-consuming (I.Gusev, X.Huang, C.Horvath., J.Chromatogr.A, 1999, 855, 273-290; Zhang, S.H., Huang, X., Zhang, J., Horváth, C., J. Chromatogr. A 2000, 877, 465-477)

Method used

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  • Raw material prescription of opposite phase anion exchange electric chromatograph integral column and preparation thereof
  • Raw material prescription of opposite phase anion exchange electric chromatograph integral column and preparation thereof

Examples

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Effect test

Embodiment 1

[0020] 1. Pretreatment of capillaries

[0021] First rinse the empty capillary column with 0.1mol / L HCl solution for about 30min, then rinse with deionized water for 10min, until the pH is equal to 7.0, rinse with 0.1mol / L NaOH for 3h, then rinse with methanol for 15min, blow dry with nitrogen and set aside . Then add a 1:1 mixture of methanol and methacryloxypropyltrimethoxysilane to the capillary treated in step 1, and react at 60°C for 24h. Then rinse with methanol for 15 min, and blow dry with nitrogen at 25°C.

[0022] 2. In-column synthesis

[0023] Isobutyl methacrylate, N-allyl dimethylamine, ethylene glycol dimethacrylate, N, N-dimethylformamide and 1,4-butanediol are respectively 12.0% by weight , 12.0%, 16.0%, 30.0%, and 30.0% were mixed, and the amount of added initiator azobisisobutyronitrile (AIBN) was 0.3% of the amount of polymer monomer. After the mixture was ultrasonically oscillated for 15 minutes, the reaction solution was Inject into a capillary of a c...

Embodiment 2

[0025] Isobutyl methacrylate, N-allyl dimethylamine, ethylene glycol dimethacrylate, N, N-dimethylformamide and 1,4-butanediol are respectively 10.0% by weight , 10.0%, 20.0%, 30.0%, and 30.0% were mixed, and the amount of added initiator azobisisobutyronitrile (AIBN) was 0.3% of the amount of polymer monomer. After the mixture was ultrasonically oscillated for 15 minutes, the reaction liquid Inject into a capillary of a certain length that has been treated according to step 1, seal both ends of the capillary, and immerse in a water bath at 60°C for 8 hours of reaction. After the reaction is complete, the column is rinsed with methanol to remove possible residual reagents in the capillary.

Embodiment 3

[0027] Isobutyl methacrylate, N-allyl dimethylamine, ethylene glycol dimethacrylate, N, N-dimethylformamide and 1,4-butanediol are respectively 10.0% by weight , 10.0%, 20.0%, 20.0%, and 40.0% were mixed, and the amount of added initiator azobisisobutyronitrile (AIBN) was 0.3% of the amount of polymer monomer. After the mixture was ultrasonically oscillated for 15 minutes, the reaction solution was Inject into a capillary of a certain length that has been treated according to step 1, seal both ends of the capillary, and immerse in a water bath at 60°C for 8 hours of reaction. After the reaction is complete, the column is rinsed with methanol to remove possible residual reagents in the capillary.

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Abstract

The invention provides a material formulation of a reversed phase ion exchange electrochromatographic column and preparation method thereof. The material contains monomers, cross-linking agent, initiator and porgenic agent. According to the material formulation, monomers are polymerized in the presence of the cross-linking agent, the porgenic agent and the initiator in a capillary to prepare the reversed phase exchange electrochromatographic column. The process of preparing the reversed phase exchange electrochromatographic column is simple and requires only one step of polymerization reaction. Since the entire column can generate positive electroosmotic flow, problems of easy trailing and non-peak during separation of basic compound can be solved. The column can also satisfy the requirement of continuous and rapid separation of neutral and ionic substances; the column has good permeability and is applicable in a buffer salt system with a high concentration. Plug burning at two ends of the column is obviated during the preparation, and difficulty on filling the column is also prevented.

Description

technical field [0001] The invention belongs to the technical field of electrochromatography, and more specifically relates to a raw material formula and a preparation method of a reversed-phase anion-exchange electrochromatographic monolithic column. Background technique [0002] Capillary electrochromatography (CEC) is a combination of capillary electrophoresis (CE) and capillary liquid chromatography (capillary-HPLC) technology. . At present, there have been many researches on special CEC stationary phases. The conventional spherical stationary phase needs to sinter the plunger at both ends of the column when filling the capillary, and the plunger is the source of bubble generation and column damage. Therefore, plunger-free column-monolithic column must be the development direction of capillary column. Monolithic columns are divided into organic polymer monolithic columns and silica-based monolithic columns according to their materials. Compared with silica monolithic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/287B01D15/36
Inventor 谢增鸿吕海霞林旭聪
Owner FUZHOU UNIV
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