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 its preparation, can solve the problems of affecting the yield and cumbersome steps, and achieve a wide application range, simple and easy-to-control process, and mild reaction conditions. Effect
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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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