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Preparation and application of hydrophilic/hydrophobic@acid/alkali equilibrium chromatography stationary phase

A chromatographic stationary phase and hydrophobic technology, applied in the field of chromatographic stationary phase, can solve the problems of unsuitability, low mechanical strength, unsuitable adsorption performance, etc., and achieve the effect of simple operation, large content and strong design

Active Publication Date: 2021-12-21
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most polymers are not suitable as stationary phases for polymer-based liquid chromatography due to their low mechanical strength and unsuitable adsorption properties.

Method used

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  • Preparation and application of hydrophilic/hydrophobic@acid/alkali equilibrium chromatography stationary phase
  • Preparation and application of hydrophilic/hydrophobic@acid/alkali equilibrium chromatography stationary phase
  • Preparation and application of hydrophilic/hydrophobic@acid/alkali equilibrium chromatography stationary phase

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Under room temperature, 2.2 g of porous silica gel, 0.84 g vinylpyridine, 1.11 g of decanoic acid, 5 ml methanol, 0.0012 g of azo diisobutyronitrile in 100 ml of round bottom flask were mixed after mixing 60 min. . The addition of 25 mL of methanol was added, and the magnetic force was stirred at 70 ° C under nitrogen protection. Finally, the product was washed with ethanol and washed with water at 70 ° C to give the affinity / hydrophobic @ acid / base balance chromatography fixed phase SIL @ Pyua. The resulting Sil @ Pyua is installed in a stainless steel column of 4.6 × 150 mm, and Sil @ Pyua column A is obtained. The chromatographic peak symmetrical symmetry of the fixed phase is good.

Embodiment 2

[0046] Under room temperature, 2.2 g of porous silica gel, 0.84 g vinylpyridine, 1.48 g of decanoic acid, 6 ml methanol, 0.0012 g of azo diisobutyronitrile in 100 ml of round bottom flask were mixed after mixing 50 min . The addition of 28 mL of methanol was added, and the magnetic force was stirred at 70 ° C under nitrogen protection. Finally, the product was washed with ethanol and washed with water at 70 ° C to give the affinity / hydrophobic @ acid / base balance chromatography fixed phase SIL @ Pyua. The resulting Sil @ Pyua is installed in a stainless steel column of 4.6 × 150 mm, and the SIL @ Pyua Column B. The retention time of column B for all analytes is improved, but the column is lower than column A.

Embodiment 3

[0048] At room temperature, 3.2 g of porous silica gel microspheres, 0.63 g of vinylpyridine, 1.11 g of umeolic acid, 4.5 ml of methanol, 0.0025 g of sodium oxidized benzoyl were mixed in a 100 mL round bottom flask. 40min . 25 ml of methanol was added, and the magnetic force was stirred and refluxed at 75 ° C under nitrogen protection. Finally, the product was washed with ethanol and washed with water at 70 ° C to give the affinity / hydrophobic @ acid / base balance chromatography fixed phase SIL @ Pyua. The resulting SIL @ Pyua is installed in a stainless steel column of 4.6 × 150 mm, and the SIL @ Pyua column C is produced. The column C is lowered with the column of columns compared to the retention time of all analytes, and the column efficacy is lower; the retention time and column efficacy of all analytes are lower than the column B.

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Abstract

The invention discloses a preparation method of a hydrophilic / hydrophobic@acid / alkali equilibrium chromatographic stationary phase. The method comprises the following steps: taking undecylenic acid and vinylpyridine as two polymer monomers, directly using a free radical initiator under the condition of not using a silanization reagent, and initiating in-situ polymerization of undecylenic acid and vinylpyridine on the surface of silica gel, and preparing hydrophilic / hydrophobic@acid / alkali equilibrium chromatographic stationary phase Sil@PyUA of undecylenic acid and vinylpyridine type polymer coated silica gel. The content of surface functional groups of the prepared Si@PyUA is large, and a large number of action sites can be provided for chromatographic separation of a sample. Chromatographic separation experiments show that the prepared hydrophilic / hydrophobic@acid / alkali equilibrium chromatographic stationary phase Sil@PyUA can be used for reversed-phase chromatographic separation of polycyclic aromatic hydrocarbons and phenol compounds; the method can also be used for hydrophilic chromatography separation of nucleoside base compounds and oxazolidinone antibiotics; and even can be used as an acid / alkali ion balance chromatographic filler for separating aromatic acid and aromatic amine compounds.

Description

Technical field [0001] The present invention relates to a method for preparing a pro- / hydrophobic @ Acid / base balance chromatography, mainly used in polycyclic aromatic hydrocarbons, phenols, nucleoside, oxazolidone antibiotics, aromatic acid, and aromatic amines It belongs to the field of chromatographic fixation. Background technique [0002] High performance liquid chromatography as one of the most commonly used separation analysis methods, is widely used in organochemical, biochemical, pharmaceutical, drug development and testing, chemical, food science, environmental monitoring, commodity inspection and judicial testing. On the one hand, the diversity of the analyte requires different characteristics of the chromatographic fixed phase, so the mixed mode column has been greatly developed. On the other hand, the difference between the same type of analyte is very small, and higher column efficiency and selectivity are required to be separated. The silica gel column excellen...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/30B01D15/20
CPCB01J20/103B01J20/264B01D15/20
Inventor 邱洪灯樊超陈佳
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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