Stationary phase of HILLIC (hydrophilic interaction chromatography) and preparation method of stationary phase

A technology of hydrophilic interaction and chromatographic stationary phase, applied in the field of chromatographic analysis, to achieve the effects of easy control of preparation conditions, good reproducibility, and cheap raw materials

Inactive Publication Date: 2017-10-20
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Polyvinylpyrrolidone (PVP) is a homopolymer with excellent properties such as solubility, low toxicity, biocompatibility, film formation, chemical stability, and physiological inertness. It is widely used in medical and health care, daily chemical industry, Food, beverage, brewing, textile printing and dyeing, new materials and other fields, but there is no relevant report about the use of polyvinylpyrrolidone (PVP) in the preparation of hydrophilic interaction chromatography stationary phase

Method used

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  • Stationary phase of HILLIC (hydrophilic interaction chromatography) and preparation method of stationary phase
  • Stationary phase of HILLIC (hydrophilic interaction chromatography) and preparation method of stationary phase
  • Stationary phase of HILLIC (hydrophilic interaction chromatography) and preparation method of stationary phase

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Example 1: Preparation of capillary liquid chromatography monolithic column

[0050] a) Capillary pretreatment: Rinse the capillary with 1.0mol / L NaOH solution for 4 hours, then rinse it with deionized water until neutral, then rinse it with methanol for 15 minutes, and dry it with nitrogen for later use; mix methanol with 3-(methacryloyloxy ) The mixed solution of propyltrimethoxysilane with a volume ratio of 1:1 is filled in the dried capillary, placed in an oven at 60°C for 12 hours, then rinsed with anhydrous methanol for 15 minutes, and blown dry with nitrogen for later use;

[0051] b) Preparation of monolithic column for capillary liquid chromatography: Weigh 150mg of N-vinylpyrrolidone, 60mg of pentaerythritol, 820mg of aqueous methanol (including 680mg of methanol and 140mg of deionized water), 1.5mg of azobisisobutyronitrile, and mix the components The chromatographic raw material is obtained, and then the chromatographic raw material is ultrasonically mixed f...

Embodiment 2

[0057] The capillary liquid chromatography monolithic column prepared in Example 1 is used as a fixed phase to carry out HILIC analysis on a mixture of toluene, acrylamide and thiourea, and the analysis conditions are:

[0058] Mobile phase A is H 2 O, mobile phase B is acetonitrile, liquid phase method: 97.5% B; Flow velocity: 800nL / min; Detection wavelength: 214nm; The obtained HILIC chromatogram is as follows figure 2 shown;

[0059] Depend on figure 2 As shown in the HILIC chromatogram, it can be seen that toluene, acrylamide, and thiourea appear from the spectrum in sequence, which shows that the efficient separation of toluene, acrylamide, and thiourea can be realized by using the capillary liquid chromatography monolithic column of the present invention as a stationary phase.

Embodiment 3

[0061] The capillary liquid chromatography monolithic column prepared in Example 1 was used as a fixed relative phenolic compound for HILIC analysis, and the analysis conditions were:

[0062] Mobile phase A is H 2 O, mobile phase B is acetonitrile, liquid phase method: 92.5% B; Flow rate: 800nL / min; Detection wavelength: 214nm; The obtained HILIC chromatogram is as follows image 3 shown;

[0063] Depend on image 3 As shown in the HILIC chromatogram, it can be seen that phenolic compounds such as toluene, phenol, pyrocatechol, resorcinol, hydroquinone, and pyrogallol appear from the spectrum in turn, which shows that the capillary liquid of the present invention The monolithic column of phase chromatography can be used as the stationary phase to achieve high-efficiency separation of phenolic compounds.

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Abstract

The invention discloses a stationary phase of HILLIC (hydrophilic interaction chromatography) and a preparation method of the stationary phase. The stationary phase of the HILLIC refers to a monolithic silica column with polyvinyl pyrrolidone bonded on the surface of porous silica gel or a monolithic capillary column with polyvinyl pyrrolidone directly bonded on the inner wall of a capillary; the monolithic capillary column comprises a capillary liquid chromatography monolithic column and a monolithic electrochromatography monolithic column. Experiments prove that the stationary phase of the HILLIC has a typical retention mechanism of hydrophilic interaction chromatography, effective separation of a series of polar compounds can be realized, efficient separation of the polar compounds can be realized without a buffer salt mobile phase, reproducibility is good, and electrochromatography column efficiency can be up to 200000 plates / m. Besides, preparation conditions of the stationary phase of the HILLIC are easy to control, raw materials are cheap and available, a preparation process is simple, and industrialization is easy to realize.

Description

technical field [0001] The invention relates to a hydrophilic interaction chromatographic stationary phase and a preparation method thereof, belonging to the technical field of chromatographic analysis. Background technique [0002] Hydrophilic Interaction Chromatography (HILIC), as a high-performance liquid chromatography technique, plays an important role in the separation and analysis of highly polar and ionic compounds such as amino acids, carbohydrates and peptides. In recent years, with the increasing demand for the separation of polar compounds in the fields of proteomics, glycomics, metabolomics and other life sciences, hydrophilic interaction chromatography has developed rapidly. [0003] As the core of chromatographic technology, the development of stationary phase materials directly affects the selectivity and separation efficiency of chromatographic separation, and restricts the application and promotion of hydrophilic interaction chromatography. There are many ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30B01D15/08
CPCB01D15/08B01J20/286B01J2220/52
Inventor 康经武邱丹叶
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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