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Modified resin for separation and purification of trilobatin and application of modified resin in lithocarpus litseifolius

A trilobatin and resin technology, applied in the field of extraction and separation of natural products, can solve the problems of large solvent consumption, long time consumption, low selectivity, etc., and achieve the effect of saving production costs and reducing the amount of resin used

Active Publication Date: 2018-06-01
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The separation method uses traditional resin, which consumes a lot of solvent, has low selectivity and takes a long time

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Add 200g of pretreated AB-8 dry resin into a three-necked bottle, add 1500mL of dichloromethane to soak and swell for 48h, then add 400g of sodium chloride, 200g of zinc chloride, and 100mL of chloromethyl methyl ether respectively, Reflux and stir at 333K for 24 hours, then wash with deionized water and methanol, and dry to obtain chloromethylated resin.

[0020] (2) Weigh 100 g of the chloromethylated resin obtained in step (1), soak it in absolute ethanol for 24 hours, wash it with distilled water until it has no alcohol smell, then soak it in 1.0M HCl for 3 hours, wash it until it is neutral, and then wash it with 1.0M NaOH Soak for 3 hours, then wash until neutral, then vacuum dry at 330K for 8 hours.

[0021] (3) The resin obtained in the step (2) was swelled in 1500mL of DMF for 48h, and the addition of quality was 300g of glucosamine hydrochloride and 200g of K 2 CO 3 . Under the condition of 353K, it was mechanically stirred at constant temperature for 2...

Embodiment 2

[0025] (1) Add 200g of pretreated AB-8 dry resin into a three-necked bottle, add 2000mL of dichloromethane to soak and swell for 24h, then add 200g of sodium chloride, 400g of zinc chloride, and 200mL of chloromethyl methyl ether respectively, Reflux and stir at 333K for 24 hours, then wash with deionized water and methanol, and dry to obtain chloromethylated resin.

[0026] (2) Weigh 100 g of the chloromethylated resin obtained in step (1), soak it in absolute ethanol for 12 hours, wash it with distilled water until it has no alcohol smell, then soak it in 1.0M HCl for 3 hours, wash it until it is neutral, and then wash it with 1.0M NaOH Soak for 3 hours, then wash until neutral, then vacuum dry at 330K for 8 hours.

[0027] (3) The resin obtained in the step (2) was swelled in 2000mL of DMF for 24h, and adding quality was 200g of glucosamine hydrochloride, quality 400g of K 2 CO 3 . Under the condition of 363K, it was mechanically stirred at constant temperature for 10h. ...

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Abstract

The invention discloses modified resin and an application thereof in separation and purification of lithocarpus litseifolius. Traditional resin is used as initial resin to be subjected to chloromethylation, the obtained resin reacts with glucosamine hydrochloride, and glucosamine modified resin is obtained. A high-purity trilobatin product is obtained through steps of drying and crushing of tenderleaves of lithocarpus litseifolius, extraction with an organic solvent, alkalization, extraction, purification of an extraction solution on a column with the glucosamine modified resin, concentrationand crystallization. The glucosamine modified resin has higher selectivity for trilobatin in lithocarpus litseifolius sweet tea and is easy to elute, the dosage of the resin is reduced, and the modified resin has better regenerability after being eluted with ethanol, and recycling is facilitated.

Description

technical field [0001] The invention relates to the technical field of extraction and separation of natural products, in particular to a resin for separation and purification and its application in Mujiangyeke. Background technique [0002] Trilobatin, (Trilobatin, CAS NO.4192-90-9), is an important flavonoid compound in Mujiangye Ketian tea, molecular formula C 21 h 24 o 10 , The relative molecular mass is 436.413, and its chemical name is 1-[4-(β-D-Glucopyranosyloxy)-2,6-dihydroxyphenyl]-3-(4-hydroxyphenyl)-1-propanone. Trilobatin belongs to dihydrochalcone compounds, which can inhibit the activity of α-glucosidase and α-amylase related to type 2 diabetes, anti-oxidation, and activity of scavenging free radicals. Its sweetness is 300 times that of sucrose . It has broad application prospects in the development of new drugs and functional foods. [0003] Patent 201510358050.1 reports "a method for the isolation of a large amount of natural sweetener trilobatin", includ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F8/32C08F8/24C08F212/08B01J20/26B01D15/08C07H15/203C07H1/08
CPCB01D15/08B01J20/265C07H1/08C07H15/203C08F8/24C08F8/32C08F212/08
Inventor 刘佳佳刘朝水刘健
Owner CENT SOUTH UNIV
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