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Preparation method and application of hydrophilic chromatographic stationary phase of cationic polysaccharide coating type

A cationic polysaccharide and hydrophilic chromatography technology, which is applied in the field of preparation of cationic polysaccharide-coated hydrophilic chromatography stationary phase, can solve the problems of affecting yield and cumbersome steps, and achieve high conversion rate, simple and easy-to-control process, and excellent reaction conditions mild effect

Inactive Publication Date: 2013-05-29
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the modified preparation method is very efficient, it also has its defects, such as the tedious steps affecting the yield, and the use of a large amount of organic reagents in the reaction process

Method used

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  • Preparation method and application of hydrophilic chromatographic stationary phase of cationic polysaccharide coating type
  • Preparation method and application of hydrophilic chromatographic stationary phase of cationic polysaccharide coating type
  • Preparation method and application of hydrophilic chromatographic stationary phase of cationic polysaccharide coating type

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add 350ml of anhydrous toluene and 23.8mL of γ-triethoxypropylmercaptosilane into a 500ml three-neck flask, heat and stir in an oil bath at 110°C, and carry out nitrogen reflux protection. Then add a particle size of 5 μm and a pore size of The specific surface area is 100m 2 g -1 20g of spherical silica particles, reacted at 110°C for 24 hours, and finished the reaction with 4 # The sand core funnel was suction filtered, washed with toluene, acetone, water and methanol in sequence, drained and dried overnight in an oven at 80°C. Next, 200 mL of 30% hydrogen peroxide solution and 60 mL of methanol solution containing 1 mL of sulfuric acid were added to the reaction intermediate product, stirred slowly at room temperature for 20 hours, washed with water and methanol, and dried to obtain sulfonated silica gel. Elemental analysis results: C1.47%, N0%, H0.78%. Add sulfonated silica gel to 1% cationic cellulose solution, the feeding ratio is 10:1, stir at room temperatu...

Embodiment 2

[0042] The chromatographic column prepared in Example 1 was used to separate sugars and sugar alcohols in the mode of hydrophilic interaction chromatography. With acetonitrile / water as the mobile phase, the volume ratio of acetonitrile and water is 80 / 20, sugar and sugar alcohols have been well separated, as shown in figure 2Shown (1 is ribose, 2 is mannitol, 3 is sucrose, 4 is maltitol, 5 is raffinose, 6 is melezitose).

Embodiment 3

[0044] The chromatographic column prepared in Example 1 was used to separate the galactooligosaccharide sample in the mode of hydrophilic interaction chromatography. Using acetonitrile / water as the mobile phase and gradient elution (water volume content: 0-60 minutes: 20-40%), the galactooligosaccharide sample was well retained and separated, such as image 3 As shown, (2 to 7 in the figure represent di-to-heptasaccharides with different degrees of polymerization respectively).

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Abstract

The invention relates to a preparation method and an application of a hydrophilic chromatographic stationary phase of a cationic polysaccharide coating type, wherein silica gel is provided with a negative charge; saccharide is of a quaternary ammonium polysaccharide provided with a positive charge. According to the preparation method, by utilizing the ionic interaction, the silica gel with a sulfonated surface and the cationic polysaccharide with the positive charge are combined in an aqueous solution system so as to prepare the agglomeration type chromatographic stationary phase. Compared with the traditional bonding sugar type stationary phase, the preparation method of the agglomeration type stationary phase is more efficient, convenient and environment-friendly. In addition, the agglomeration type stationary phase has good separation selectivity, repeatability and stability, thereby having the great application potentiality for the separation of polar compounds of other types. Therefore, the agglomeration type stationary phase can be widely applied to glycobiology and glycoproteomics.

Description

【Technical field】 [0001] The invention relates to the technical field of hydrophilic chromatographic stationary phase, in particular to a preparation method and application of a cationic polysaccharide-coated hydrophilic chromatographic stationary phase. 【Background technique】 [0002] Hydrophilic interaction chromatography was first proposed by Alpert [A.J.Alpert, J.Chromatogr.A, 1990, 499, 177], and it is one of the hot spots in the field of chromatography in recent years. Because of its strong retention and good separation selectivity for polar compounds, as well as its good compatibility and sensitivity with mass spectrometry, its applications are becoming more and more extensive, and it has attracted more and more attention. [0003] With the modification of the surface of silica gel, sugars on the surface of silica gel have also been developed rapidly as a new type of hydrophilic chromatography stationary phase [P.Hemstrom, et al, J.Sep.Sci, 2006, 29, 1784]. The glyc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30B01D15/08
Inventor 梁鑫淼柯燕雄盛骞莹
Owner EAST CHINA UNIV OF SCI & TECH
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