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Bonding polysaccharide type hydrophilic chromatographic stationary phase as well as preparation method and application thereof

A technology of hydrophilic chromatography and stationary phase, which is applied in the field of new liquid phase hydrophilic chromatography stationary phase and preparation, can solve the problems of affecting yield and cumbersome steps, and achieve a wide application range, simple and easy-to-control process, and high conversion rate Effect

Inactive Publication Date: 2015-06-24
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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  • Bonding polysaccharide type hydrophilic chromatographic stationary phase as well as preparation method and application thereof
  • Bonding polysaccharide type hydrophilic chromatographic stationary phase as well as preparation method and application thereof
  • Bonding polysaccharide type hydrophilic chromatographic stationary phase as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Add 320ml of anhydrous toluene and 32mL of 3-aminopropyltriethoxysilane 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 300m 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, and dried in an oven at 80°C overnight. The elemental analysis results of the product: C5.36%, N1.56%, H1.22%. Next, 120 mL of anhydrous dioxane solution containing 7.8 g of carbonyldiimidazole was added to the reaction intermediate product, stirred slowly at room temperature for 4 hours, washed with anhydrous dioxane solution and methanol, and dried. The elemental analysis results of the product: C8.42%, N3.34%, H1.48%. Add the product to 1% dextran aqueous solution, the molecular weight o...

Embodiment 2

[0044] The chromatographic column prepared in Example 1 was used to separate sugars and sugar alcohols in the mode of hydrophilic interaction chromatography. Using acetonitrile / water as the mobile phase, the volume ratio of acetonitrile and water is 80 / 20, sugars and sugar alcohols are well separated, as shown in figure 2 Shown (1 is ribose, 2 is mannitol, 3 is sucrose, 4 is maltitol, 5 is raffinose, 6 is melezitose).

Embodiment 3

[0046] 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, under the condition of gradient elution (water volume content: 0-60 minutes: 20-40%), the galactooligosaccharide sample has been 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 bonding polysaccharide type hydrophilic chromatographic stationary phase as well as a preparation method and an application thereof. A structure of the bonding polysaccharide type hydrophilic chromatographic stationary phase is shown in the specification, wherein SiO2 is silica gel, saccharide is polysaccharide with molecular weight ranging from hundreds to tens of thousands. The invention provides the preparation method of the stationary phase material, wherein the preparation method comprises the following step: modifying the surface of the silica gel and bonding with the polysaccharide in an aqueous liquor system by taking carbonyl dimidazole (CDI) as a connecting arm to prepare the bonding polysaccharide type chromatographic stationary phase. Compared with the conventional bonding saccharide type stationary phase preparation method, the stationary phase preparation method disclosed by the invention is more efficient, convenient and environment-friendly. And meanwhile, the bonding polysaccharide type hydrophilic chromatographic stationary phase has good separating selectivity, repeatability and stability, has great application potentiality in separating polar compounds of other types, and is widely applied in saccharide separating and saccharide-modifying proteomics.

Description

【Technical field】 [0001] The present invention relates to a novel liquid-phase hydrophilic chromatographic stationary phase and a preparation method thereof, specifically, a preparation method of a bonded polysaccharide-type hydrophilic chromatographic stationary phase which utilizes a special connecting arm to bond polysaccharides to the surface of silica gel and application. 【Background technique】 [0002] Hydrophilic interaction chromatography [A.J.Alpert, J. Chromatogr.A, 1990, 499, 177] has strong retention and good separation selectivity for polar compounds, and good compatibility and sensitivity with mass spectrometry, etc. It is one of the hot spots in the field of chromatography research in recent years. With its high development and attention, more and more new hydrophilic chromatographic stationary phases have also been developed rapidly. [0003] As the most widely used stationary phase material, silica gel is a very feasible means to modify its surface for sep...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01J20/30B01D15/08C08G83/00C07K16/06C07K1/22
Inventor 梁鑫淼柯燕雄盛骞莹
Owner EAST CHINA UNIV OF SCI & TECH
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