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1,2,3,4,6-O-pentagalloylglucose molecular imprinting monolithic column preparation method

A pentagalloylglucose, molecular imprinting technology, applied in separation methods, chemical instruments and methods, solid adsorbent liquid separation, etc., can solve problems such as unachievable purity

Active Publication Date: 2017-06-30
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the purity of the 1,2,3,4,6-O-pentagalloyl glucose separated and purified by this molecular imprinting method cannot meet the requirements of the standard (purity greater than or equal to 98%)

Method used

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  • 1,2,3,4,6-O-pentagalloylglucose molecular imprinting monolithic column preparation method
  • 1,2,3,4,6-O-pentagalloylglucose molecular imprinting monolithic column preparation method
  • 1,2,3,4,6-O-pentagalloylglucose molecular imprinting monolithic column preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Preparation of 1,2,3,4,6-O-pentagalloyl glucose molecularly imprinted monolithic column by in situ polymerization:

[0021] a. Dissolve 47.04 mg of 1,2,3,4,6-O-pentagalloyl glucose and 32 μL of 4-vinylpyridine in 240 μL of ternary porogen N,N-dimethylformamide, dimethyl sulfoxide 1200 μL and 2468 μL of 1-butyl-3-methyltetrafluoroborate, then add 8.84 mg of nickel acetate and 20 mg of free radical initiator azobisisobutyronitrile, then add 630 μL of ethylene glycol dimethacrylate and 171.5 μL of methyl ether methacrylate oligomer with an average relative molecular mass of 300 g / mol, ultrasonicated for 30 minutes to completely dissolve and mix all components to obtain a homogeneous solution, then fill the solution with nitrogen gas to remove the dissolved The oxygen in it is transferred to the stainless steel tube, and the two ends of the stainless steel tube are sealed, and the stainless steel column is placed in a constant temperature water bath with a temperature of 60...

Embodiment 2

[0025] Preparation of 1,2,3,4,6-O-pentagalloyl glucose molecularly imprinted monolithic column by in situ polymerization:

[0026] a. Dissolve 28.22 mg of 1,2,3,4,6-O-pentagalloyl glucose and 32 μL of 4-vinylpyridine in 240 μL of ternary porogen N,N-dimethylformamide, dimethyl sulfoxide 1200 μL and 2468 μL of 1-butyl-3-methyltetrafluoroborate, then add 8.84 mg of nickel acetate and 20 mg of free radical initiator azobisisobutyronitrile, then add 630 μL of ethylene glycol dimethacrylate and The average relative molecular weight is 300g / mol methyl ether methacrylate oligomer 171.5μL, sonication for 30 minutes, so that all components are completely dissolved and mixed to obtain a homogeneous solution, and then the solution is filled with nitrogen to remove the dissolved oxygen, transfer the solution to a stainless steel tube, and seal both ends of the stainless steel tube, and put the stainless steel column into a constant temperature water bath at a temperature of 60°C for 18 ho...

Embodiment 3

[0030] Preparation of 1,2,3,4,6-O-pentagalloyl glucose molecularly imprinted monolithic column by in situ polymerization:

[0031] a. Dissolve 14.12 mg of 1,2,3,4,6-O-pentagalloyl glucose and 32 μL of 4-vinylpyridine in 240 μL of ternary porogen N,N-dimethylformamide, dimethyl sulfoxide 1200 μL and 2468 μL of 1-butyl-3-methyltetrafluoroborate, then add 8.84 mg of nickel acetate and 20 mg of free radical initiator azobisisobutyronitrile, then add 630 μL of ethylene glycol dimethacrylate and 171.5 μL of methyl ether methacrylate oligomer with an average relative molecular mass of 300 g / mol, ultrasonicated for 30 minutes to completely dissolve and mix all components to obtain a homogeneous solution, and then fill the solution with nitrogen gas to remove the dissolved Oxygen in it, transfer the solution to a stainless steel tube, and seal both ends of the stainless steel tube, put the stainless steel column in a constant temperature water bath with a temperature of 60°C for 18 hou...

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Abstract

The present invention relates to a 1,2,3,4,6-O-pentagalloylglucose molecular imprinting monolithic column preparation method, which comprises: using 1,2,3,4,6-O-pentagalloylglucose as a template molecule, using a ternary pore forming agent N,N-dimethylformamide, dimethyl sulfoxide and 1-butyl-3-methyl tetrafluoroborate as a solvent, adding a functional monomer, a cross-linking agent, metal ions, a methyl ether methacrylate oligomer and an initiator, carrying out ultrasonic dissolution, inflating nitrogen, removing dissolved oxygen, and carrying out a polymerization reaction in a water bath so as to finally obtain the 1,2,3,4,6-O-pentagalloylglucose molecular imprinting monolithic column having selectivity. According to the present invention, the imprinting factor of the method can be up to 73.9, the method can be used for solid phase extraction, and the selective purification of the 1,2,3,4,6-O-pentagalloylglucose can be achieved; and the printing polymer has characteristics of simple preparation and good durability, and can be adopted as the solid phase extraction filler so as to provide the effect method for the separation and purification of the 1,2,3,4,6-O-pentagalloylglucose (the purity is greater than 98%).

Description

technical field [0001] The invention relates to a preparation method of a 1,2,3,4,6-O-pentagalloyl glucose molecularly imprinted monolithic column. It shows good selectivity and specificity, and can be used for the separation and purification of 1,2,3,4,6-O-pentagalloyl glucose. Background technique [0002] 1,2,3,4,6-O-Pentagalloyl Glucose is a polyphenolic monomer compound, which has various biological and pharmacological properties such as anti-oxidation, anti-inflammation, antagonism of endotoxin, anti-cancer, and treatment of diabetes learning activity. Therefore, 1,2,3,4,6-O-pentagalloylglucose has a good application prospect in the field of medicine and health care. However, due to the low content of 1,2,3,4,6-O-pentagalloylglucose in plants, if the traditional method is used for purification and separation, it will be time-consuming, laborious and inefficient; if it is purified and separated by preparative liquid chromatography, due to The equipment is expensive a...

Claims

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Application Information

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IPC IPC(8): C08F222/14C08F226/06B01D15/20B01J20/26B01J20/285B01J20/30
CPCB01D15/20B01J20/268B01J20/285C08F222/14C08J9/26C08J9/28C08J2201/0422C08J2335/02C08F226/06
Inventor 刘照胜王超阿吉艾克拜尔·艾萨
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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