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Capillary electrochromatographic open tubular column with mixed effect of hydrophilia and ion exchange and preparation method of same

A technology of capillary electrochromatography and ion exchange, which is applied in separation methods, chemical instruments and methods, material separation, etc., can solve the problems of irreversible adsorption of silanol and difficult separation, achieve a wide range of separation objects, a wide range of pH applications, and avoid The effect of technical difficulties

Inactive Publication Date: 2011-05-25
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problem of irreversible adsorption and difficult separation of silanol on the capillary column for polar alkaline substances, the present invention provides a hydrophilic-ion exchange mixed action capillary electrochromatographic open-tubular column and its preparation method. On-column polymerization of silanized, ionic and polar monomers

Method used

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  • Capillary electrochromatographic open tubular column with mixed effect of hydrophilia and ion exchange and preparation method of same
  • Capillary electrochromatographic open tubular column with mixed effect of hydrophilia and ion exchange and preparation method of same

Examples

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Effect test

Embodiment 1

[0020] Example 1: Preparation of Hydrophilic-Ion Exchange Mixed Action Capillary Electrochromatography Open-Tube Column by Column Polymerization

[0021] 1. Pretreatment: Rinse the capillary empty column with 1-6mol / L HCl solution for about 15-30min, then rinse it with deionized water for 10-15min, then rinse it with 0.1-1mol / L NaOH for 30min, then wash it with 0.1-1mol / L Rinse with HCl solution, then rinse with deionized water for 10 to 15 minutes, rinse with methanol for 15 to 30 minutes, and blow dry with nitrogen for use.

[0022] 2. Silanization treatment: add 0.05% to 0.5% (w / v) Inhibitor 2,2-diphenyl-1-picrylhydrazine, react at 110°C for 12h-24h; then rinse with methanol for 15min-30min; dry with nitrogen at 50-70°C.

[0023] 3. In-column synthesis: mix according to the above formula, ultrasonically vibrate the resulting mixture for 10-15 minutes, blow nitrogen to remove dissolved oxygen in the mixture, then inject the mixture into the treated capillary, seal both end...

Embodiment 2

[0024] Example 2: Hydrophilic-ion exchange mixed action capillary open-tubular column for separation of alkaloids

[0025] Apply the hydrophilic-ion exchange mixed action capillary open-tubular column of the present invention (inner diameter 50mm, total length 60.0cm, effective length 40.0cm), with acetonitrile: phosphate (pH 4.5 10mM) = 4: 6 is the buffer solution as the mobile phase, Separation voltage +16kV, under the CEC anode electroosmotic flow mode, the three alkaloids of berberine hydrochloride, tetrahydrochloride and protoopine were separated by capillary electrochromatography-ultraviolet detection, and the alkaloids were completely separated under the above conditions. Such as figure 1 As shown, the elution peaks are: a. berberine hydrochloride; b. tetrahydropalmatine; c. proto-opioid, which reduces the tailing phenomenon caused by the adsorption of alkaloids.

Embodiment 3

[0026] Example 3: Hydrophilic-ion exchange mixed action capillary open-tubular column separation of quinolones

[0027] Apply the hydrophilic-ion exchange mixed action capillary open-tubular column of the present invention (inner diameter 50mm, total length 60.0cm, effective length 40.0cm), with acetonitrile: phosphate (pH 7.0 10mM)=5: 5 is the mobile phase as the buffer solution, Separation voltage +10kV, under CEC anode electroosmotic flow mode, separate 7 quinolone antibiotics, such as figure 2 shown. The elution peaks are: sparfloxacin, gatifloxacin, enoxacin, ofloxacin, pefloxacin, fleroxacin, pazufloxacin, quinolones achieved baseline separation under the above conditions .

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Abstract

The present invention discloses a capillary electrochromatographic open tubular column with a mixed effect of hydrophilia and ion exchange and a preparation method of the same. The convergence layer of the open tubular column comprises methyl methacrylate ionic monomers, 2-methyl-3-butene cyanide polar monomers, initiators and cross-linking agents, wherein the ionic monomers account for 3.5-7.0 percent by weight, the polar monomers account for 8.0-27.0 percent by weight, the cross-linking agents account for 3.5-7.0 percent by weight, the initiators account for 0.3-1.0 percent by weight, the inert solvents account for 60.0-90.0 percent by weight. The bonded cyano structure in the open tubular column has a function of hydrophilic chromatography, carboxyl groups can be dissociated to generate a positive electroosmotic flow, ion exchange can occur between the carboxyl groups and basic amino positive charges, and the problems that polar alkaline materials are absorbed on a capillary column irreversibly and cannot be separated easily are solves under the combined effect of the carboxyl groups and the basic amino positive charges. The functional coating of the polar capillary open tubular column is modified via chemical bonding, and the open tubular column has a mixed mode of hydrophilic chromatography and ion exchange, has a good effect on separation of positive charge type alkaline drugs, has good reproducibility, and is suitable for capillary electrochromatographic separation and analysis of polar drugs.

Description

Technical field: [0001] The invention relates to a hydrophilic-ion exchange mixed action capillary electrochromatography open-tubule column and a preparation method thereof, belonging to the technical field of capillary electrochromatography. Background technique: [0002] Capillary electrochromatography (capillary electrochromatography) is an efficient and fast new chromatographic micro-separation technology developed in recent years. As one of the main types of capillary chromatographic columns, capillary open-tubular column has the characteristics of simple preparation, no need for plunger, high efficiency and fast separation column, and has been valued by chromatographic workers. [0003] Capillary electrochromatographic open-tube columns are divided into two types: physical adsorption and chemical bonding modification. Among them, the preparation method of the physical adsorption type open-tubular column is simple, but unstable, and the coating needs to be renewed cont...

Claims

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Application Information

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IPC IPC(8): G01N30/96
CPCB01D15/3847B01D15/305B01D15/3885B01D15/363
Inventor 林旭聪谭静静周孙英谢增鸿
Owner FUZHOU UNIV
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