Syringin imprinted monolithic column preparation method

A technology of syringin and monolithic column, which is applied in the field of preparation of syringin imprinted monolithic column, can solve the problems of complex operation, cumbersome preparation process, and low purity, and achieve the effect of simple synthesis process, good MIPs performance, and low cost

Active Publication Date: 2021-01-29
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

CN108912186A reported that by drying the Chinese herbal medicine Ilex chinensis, pulverizing, sieving, solvent reflux, decolorizing and filtering impurities, and finally crystallizing and refining to obtain a syringin sample with high content, but the operation is complicated and the purity is not high
CN106188173A reported that the extract was made of macroporous resin, eluted with 70% ethanol, followed by silica gel chromatography, eluted with ethyl acetate, and then recrystallized with ice ethanol / water to obtain syringin with a purity of 90-98% , the preparation process of this method is also cumbersome
The research and application of deep eutectic solvents are still in the stage of laboratory research

Method used

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  • Syringin imprinted monolithic column preparation method
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  • Syringin imprinted monolithic column preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Preparation of syringin imprinted monolithic column by in situ polymerization:

[0022] a. heating choline chloride and itaconic acid in a molar ratio of 1.5:1 in an oil bath at a temperature of 90°C for 60 minutes to obtain choline chloride-itaconic acid;

[0023] b. Dissolve 1.14% of syringin and 4.80% of choline chloride-itaconic acid obtained in step a in 12.05% of methanol, then add 0.46% of azobisisobutyronitrile, and then add dimethacrylic acid Ethylene glycol ester 21.84%, 1-butyl-3-methylimidazolium tetrafluoroborate 54.09%, isopropanol 2.38% and polyethylene glycol 400 3.25%, sonicate for 30 minutes to dissolve all components and mix well , to obtain a homogeneous solution, and then flush nitrogen in the solution to remove dissolved oxygen. After the solution is clarified, transfer the solution to a stainless steel column, quickly seal both ends of the stainless steel column, and react in a water bath at a temperature of 60°C 12 hours;

[0024] c. Take the s...

Embodiment 2

[0027] Preparation of syringin imprinted monolithic column by in situ polymerization:

[0028] a. heating choline chloride and itaconic acid in a molar ratio of 1.5:1 in an oil bath at a temperature of 90°C for 60 minutes to obtain choline chloride-itaconic acid;

[0029] b. Dissolve 0.50% of syringin and 4.84% of choline chloride-itaconic acid obtained in step a in 12.13% of methanol, then add 0.46% of azobisisobutyronitrile, and then add dimethacrylic acid Ethylene glycol ester 21.96%, 1-butyl-3-methylimidazolium tetrafluoroborate 54.44%, isopropanol 2.41% and polyethylene glycol 400 3.26%, sonication for 30min, so that all components are completely dissolved and mixed , to obtain a homogeneous solution, and then flush nitrogen in the solution to remove dissolved oxygen. After the solution is clarified, transfer the solution to a stainless steel column, quickly seal both ends of the stainless steel column, and place it in a water bath at a temperature of 60°C Reaction for 1...

Embodiment 3

[0033] Preparation of syringin imprinted monolithic column by in situ polymerization:

[0034] a. heating choline chloride and itaconic acid in a molar ratio of 1.5:1 in an oil bath at a temperature of 90°C for 60 minutes to obtain choline chloride-itaconic acid;

[0035] b. Dissolve 1.18% of syringin and 5.00% of choline chloride-itaconic acid obtained in step a in 12.51% of methanol by mass percentage, then add 0.48% of azobisisobutyronitrile, and then add dimethacrylic acid Ethylene glycol ester 18.83%, 1-butyl-3-methylimidazolium tetrafluoroborate 56.16%, isopropanol 2.49% and polyethylene glycol 400 3.36%, sonication for 30min, so that all components are completely dissolved and mixed , to obtain a homogeneous solution, and then flush nitrogen in the solution to remove dissolved oxygen. After the solution is clarified, transfer the solution to a stainless steel column, quickly seal both ends of the stainless steel column, and place it in a water bath at a temperature of 6...

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Abstract

The invention relates to a syringin imprinted monolithic column preparation method, which comprises: adopting syringin as a template, adding polyethylene glycol 400, isopropanol and methanol to dissolve the template, adopting eutectic solvent choline chloride itaconic acid as a functional monomer, adding cross-linking agent ethylene glycol dimethacrylate, porogenic agent 1-butyl -3 -methyl imidazole tetrafluoroborate and initiator azo diisobutyronitrile, and carrying out a polymerization reaction to obtain the syringin molecularly imprinted monolithic column with selectivity. According to themethod, the eutectic solvent choline chloride itaconic acid is used as the functional monomer, compared with use of a traditional functional monomer 4-vinylpyridine, the method is green and environmentally friendly, meanwhile, the syringin imprinting cost is reduced, the syringin imprinting monolithic column and a blank control column are successfully synthesized in a stainless steel tubular column, and chromatographic condition optimization is conducted on the syringin imprinting monolithic column. Experimental results show that the maximum imprinting factor can reach 3.11. The method is simple in preparation, the syringin imprinted monolithic column is good in durability, and a cost-saving method is provided for separation and purification of syringin.

Description

technical field [0001] The invention relates to a preparation method of a syringin imprinted monolithic column using a deep eutectic solvent as a functional monomer. The imprinted polymer exhibits good selectivity to syringin and can be used for the separation and purification of syringin. Background technique [0002] Syringa is a phenylpropanol glycoside compound. Pharmacological studies in recent years have shown that it is a strong anti-hepatotoxic drug, which can restore the enzyme activity of the microsomal enzyme system and inhibit lipid peroxidation, and can promote liver function. Toxin metabolism, and improve liver function, make it normal, so syringin has great medicinal value, the market demand for syringin is greater. Because the content of syringin in plants is low and cannot be used directly, how to obtain high-purity syringin is particularly important. [0003] At present, the traditional methods for separating, preparing and purifying syringin mainly includ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/285C08F222/14C08F222/22C08J9/26
CPCB01J20/268B01J20/285C08F222/102C08J9/26C08F222/22
Inventor 黄艳萍张雪杨建刘照胜阿吉艾克拜尔·艾萨
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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