Restricted access type chiral chromatography MC (monolithic column) as well as preparation method and application thereof

A technology of chiral chromatography and monolithic column, which is applied in separation methods, chemical instruments and methods, and other chemical processes. Effects on Chromatographic Efficiency

Inactive Publication Date: 2015-11-18
CHINA PHARM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation of organic monolithic columns mostly adopts the free radical polymerization method, while the traditional free radical polymerization reaction has the disadvantages that the process is not easy to control and the molecular weight distribution of the product is large.

Method used

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  • Restricted access type chiral chromatography MC (monolithic column) as well as preparation method and application thereof
  • Restricted access type chiral chromatography MC (monolithic column) as well as preparation method and application thereof
  • Restricted access type chiral chromatography MC (monolithic column) as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039]Preparation of monolithic column MC: NPMA (1.41 mmol, 292 mg) and EGDMA (1.41 mmol, 266 microliters) were added to AIBN (4.7 micromoles, 0.77 mg), PMDETA (18.8 micromoles, 4.0 microliters) and In the mixture of copper bromide (9.4 micromole, 2.1 mg) in 4 ml of acetonitrile / lauryl alcohol (9 / 1, v / v), the air in the solution was replaced by high-purity nitrogen gas, and it was injected into the stainless steel chromatographic empty column Medium (150mm x 4.6mm), sealed. React for 24 hours under 80°C water bath condition. The obtained MC monolithic column was connected to the liquid chromatography pump and rinsed with methanol.

Embodiment 2

[0041] Preparation of β-cyclodextrin-modified monolithic column CD-MC: connect monolithic column MC to a liquid chromatography pump, and elute with methanol / water (1 / 9, v / v) for 30 minutes. Then the sodium carbonate buffer solution (pH 11, ion concentration 60 mmol / L) containing β-CD (17 mmol / L) was injected into the chromatographic monolithic column in a fluid manner. The reaction was carried out at 50°C for 4 hours, and the above process of elution, injection of β-cyclodextrin and heating reaction was repeated three times. Finally, methanol / water (1 / 1, v / v) was used as mobile phase to remove reaction by-products and unreacted reagents. From scanning electron microscope images ( figure 2 ), it can be seen that the polymer particles are regular and the size of the through holes between the particles is about 0.5 micron, which has good permeability and porosity.

Embodiment 3

[0043] The preparation of limited entry chiral monolithic column RA-CD-MC: will contain HEMA (0.5 mmol / liter), BIBB (6.25 micromol / liter), cuprous bromide (5 micromol / liter) and PMDETA (10 micromol / liter) of methanol solution, through high-purity nitrogen deoxygenation, packed into a 250 mm × 4.6 mm stainless steel chromatographic column, connected to the HPLC infusion pump, and connected to the CD-MC monolithic column at the outlet of the stainless steel column. After 20 minutes of infusion with methanol as the mobile phase, the CD-MC monolithic column was removed and sealed. The reaction was heated in a water bath at 60°C for 4 hours. Finally, methanol was used as the mobile phase to wash the obtained RA-CD-MC monolithic column.

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Abstract

The invention discloses a restricted access type chiral chromatography MC (monolithic column) as well as a preparation method and an application thereof. The preparation process of the restricted access type chiral chromatography MC comprises steps as follows: (1), a framework of the chromatography MC is prepared with an RATRP (reverse atom transfer radical polymerization) method; (2), beta-CD (beta-cyclodextrin) is modified on the framework of MC to serve as a chiral selector; (3),DATRP (direct atom transfer radical polymerization) is initiated by active sites on the surface of the framework of the MC, and a hydrophilic restricted access layer is grafted. The restricted access type chiral chromatography MC has the advantages that the MC can be applied to direct injection analysis of biological samples, has high stability and is suitable for quick separation analysis of chiral drugs.

Description

technical field [0001] The invention belongs to the field of chromatographic stationary phases of organic polymer materials, and in particular relates to a limited-advance chiral chromatographic monolithic column prepared by atom transfer radical polymerization and its preparation method and application. Background technique [0002] The matrix components in biology are complex, such as serum, plasma and urine samples must be pretreated before high performance liquid chromatography (HPLC) analysis, because biological macromolecules such as proteins and nucleic acids in biological samples encounter hydrophobic When using a non-reversed phase chromatography packing material, the structure will change, leading to its denaturation and adsorption on the surface of the chromatography packing material, resulting in the clogging of the porous packing material and the reduction of column efficiency, which will seriously interfere with the determination of small molecule analytes. As ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/29B01J20/30B01D15/38G01N30/60
Inventor 王怀松冯夏奕魏纪平
Owner CHINA PHARM UNIV
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