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Polymer monolithic column, and preparation method and application thereof

A polymer, monolithic column technology, applied in the field of liquid chromatography, to achieve the effect of many action sites, easy operation and low column back pressure

Inactive Publication Date: 2012-10-24
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As the stationary phase of the silica gel packed column, it has played the role of ion exchange and reversed phase multi-mode, therefore, it is an ideal material for modifying the monolithic column with multi-mode, and so far there is no research on ionic liquid modified monolithic column for HPLC separation to report

Method used

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  • Polymer monolithic column, and preparation method and application thereof
  • Polymer monolithic column, and preparation method and application thereof
  • Polymer monolithic column, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Glycidyl methacrylate, ethylene glycol dimethacrylate, cyclohexanol, dodecanol, and azobisisobutyronitrile are respectively 18.0%, 17.6%, 56.5%, 6.9%, and 1.0% by weight Mixed, purged with nitrogen to remove oxygen, ultrasonicated for 10 minutes, poured into a stainless steel column tube with a syringe, sealed at both ends, and polymerized in a water bath at 60°C for 24 hours. The polymerized column was flushed with 100 mL of methanol into the porogen to obtain a blank chromatographic monolithic column. Normal experiments were performed after the cartridge had equilibrated for one hour with the mobile phase running.

Embodiment 2

[0035] Glycidyl methacrylate, ethylene glycol dimethacrylate, cyclohexanol, dodecanol, and azobisisobutyronitrile are respectively 18.0%, 17.6%, 56.5%, 6.9%, and 1.0% by weight Mixed, purged with nitrogen to remove oxygen, ultrasonicated for 10 minutes, poured into a stainless steel column tube with a syringe, sealed at both ends, and polymerized in a water bath at 60°C for 24 hours. The polymerized column was flushed with 100 mL of methanol as a porogen, and then the epoxy group on the surface of the whole column was hydrolyzed with 0.25 M dilute sulfuric acid at 60°C for 4 hours. 40 mL of an aqueous solution of 1-butyl-3-vinylimidazolium chloride was passed through the column for 13 hours, and the temperature was controlled at 80°C. The grafted column body is washed with water to obtain a chromatographic monolithic column with a mixed separation mode. Finally the column was equilibrated with the mobile phase running for one hour for normal experiments.

Embodiment 3

[0036] Embodiment 3, separation experiment:

[0037] 1

[0038] Using the monolithic column in Example 2 as the stationary phase, VB1, VB3, and VB9 were separated in anion exchange mode. Use 20.0mM pH7.0 phosphate buffer as mobile phase A, the above phosphate buffer containing 1.0M sodium chloride as mobile phase B, gradient elution: 0 minutes, 3% B; 4.49 minutes, 3% B; 4.50 minutes , 50%B; flow rate, 1.0mL / min; UV detection wavelength, 254nm.

[0039] The obtained chromatogram is as figure 1 As shown in the curve a, it can be seen from the figure that the three vitamin B substances have been basically separated, and the order of the peaks is: VB1, VB3, and VB9.

[0040] 2

[0041] Using the monolithic column in Example 1 as the stationary phase, VB1, VB3, and VB9 were separated in anion exchange mode. Use 20.0mM pH7.0 phosphate buffer as mobile phase A, the above phosphate buffer containing 1.0M sodium chloride as mobile phase B, gradient elution: 0 minutes, 3% B; 4.49 m...

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Abstract

The invention discloses a polymer monolithic column, and a preparation method and application thereof. The monolithic column is prepared from the raw materials consisting of monomers, a cross-linking agent, a pore forming agent, an initiator and post-modification functional monomers through the following steps: subjecting polymer fluid prepared according to a raw materials formula to polymerization in a stainless steel cylindrical tube, rinsing the monolithic column with methanol and carrying out a grafting reaction of the functional monomers on the surface of the column in the presence of the initiator so as to obtain a chromatographic column capable of anion exchange and phase reversal. According to the invention, the preparation method is simple and is easy to operate; respective separation of acidic, alkali and neutral substances under two modes is realized through adjusting a mobile phase of liquid chromatogram, and therefore, an application scope of the monolithic column is broadened and a novel idea for development of the column is provided.

Description

technical field [0001] The invention belongs to the technical field of liquid chromatography, and more specifically relates to a polymer monolithic column and its preparation method and application. Background technique [0002] Polymer monolithic columns are a class of monolithic materials that appeared in the 1990s and have the advantages of in-situ preparation, good permeability, and convective mass transfer. They are widely used in material separation, enzyme reactors, and catalytic media. As the separation medium of high performance liquid chromatography, the performance of polymer monolithic column is mainly restricted by two factors: skeleton structure and surface chemical properties. Its skeleton structure can obtain excellent column morphology by changing the polymerization method, adjusting the polymerization temperature, changing the composition of the porogen and the content of the crosslinking agent; and its surface chemical properties can usually be obtained by...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/281B01J20/30
Inventor 齐莉李雅萍沈莹张海枝
Owner INST OF CHEM CHINESE ACAD OF SCI
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