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Production process for jointly separating high-purity liquiritin, bitterness-removed glycyrrhizin and glycyrrhiza uralensis fisch total flavonoids from mono-ammonium glycyrrhizinate mother liquor paste

A technology of monoammonium glycyrrhizinate and total flavonoids of licorice, which is applied in the fields of food and medicine, can solve the problems of high production cost, complicated technical process, and effective utilization of raw materials, and achieve low production cost, good product safety, and increased product additional value. value effect

Active Publication Date: 2021-01-12
高颖
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The same production costs are high and there is no market competitiveness
[0010] Dalian Institute of Physical Chemistry, Chinese Academy of Sciences has applied for a patent named "A Preparation Method of Liquiritin" (application number: 200710011041.0). Porous resin, high-efficiency industrial chromatographic column separation, and freeze-drying to obtain liquiritin. This process is complex, requires high equipment, difficult operation, and takes a long time. It is not suitable for large-scale industrial production.
[0011] To sum up, the existing technical process is complicated, the equipment requirements are high, the operation is difficult, the use of various organic solvents that may cause safety hazards, the raw materials are not fully and effectively utilized, the added value is low, and the production cost is relatively high. shortcoming

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1, a production process for jointly separating high-purity liquiritin, debittering glycyrrhizin and total flavonoids from glycyrrhizinate monoammonium salt mother liquor paste, taking 1 kg of glycyrrhizinate monoammonium salt mother liquor paste powder in a reaction kettle , add 4L pure water, adjust the pH to 8, dissolve, and the dissolved solution is subjected to 1# polyamide column chromatography. inner resin volume) to obtain the eluent; adjust the pH of the eluent to 6, then go through 2# polyamide column chromatography, elute with 2BV pure water and collect the eluate for later use, and then 2# polyamide The column was eluted sequentially with 2BV 20% ethanol and 2BV 40% ethanol, and detected by TLC. The eluent containing high content of liquiritin was combined and concentrated under reduced pressure at 70°C to obtain 501 g of crude liquiritin; Heat at ℃ until just dissolved, filter, place the filtrate to crystallize, filter, dry, and recrystallize to obta...

Embodiment 2

[0025] Example 2, a production process for the joint separation and preparation of high-purity glycyrrhizin, debittering glycyrrhizin and total flavonoids of glycyrrhizinate from monoammonium glycyrrhizinate mother liquor paste, taking 1 kg of ammonium glycyrrhizinate mother liquor paste powder in a reaction kettle, Add 2L of pure water to adjust the pH to 9, and the dissolved solution is subjected to 1#D101 column chromatography, the mass ratio of the loading sample to 1#D101 resin is 1:8, and eluted with 4BV pure water to obtain the eluate; Adjust its pH to 4, then go through 2# polyamide column chromatography, elute with 3BV pure water and collect the eluate for later use, then 2# polyamide column is eluted with 4BV 10% ethanol and 2BV 30% ethanol in sequence, TLC detection, combined eluent containing high content of liquiritin, concentrated under reduced pressure at 70°C to obtain 472g of crude liquiritin; added 3L of 95% ethanol to the crude product, heated at 75°C until j...

Embodiment 3

[0028]Example 3, a production process for the joint separation and preparation of high-purity glycyrrhizin, debittering glycyrrhizin and total flavonoids of glycyrrhizinate from monoammonium glycyrrhizinate mother liquor paste, taking 1 kg of ammonium glycyrrhizinate mother liquor paste powder in a reaction kettle, Add 3L of pure water to adjust the pH to 8.0. After dissolving, go through 1#LX-392 column chromatography, the mass ratio of the loading sample to 1#LX-392 resin is 1:6, and elute with 4BV pure water to obtain the eluted solution; adjust its pH to 5, and then go through 2# polyamide column chromatography, elute with 4BV pure water and collect the eluate, then wash the 2# polyamide column with 3BV 20% ethanol and 3BV30% ethanol in sequence Removed, TLC detection, combined eluent containing high content of liquiritin, concentrated under reduced pressure at 70°C to obtain 453g of crude liquiritin; added 4L of 95% ethanol to the crude product, heated at 75°C until just d...

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PUM

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Abstract

The invention discloses a production process for jointly separating high-purity liquiritin, bitterness-removed glycyrrhizin and glycyrrhiza uralensis fisch total flavonoids from mono-ammonium glycyrrhizinate mother liquor paste. The production process comprises the following steps that (1) the mono-ammonium glycyrrhizinate mother liquor paste is taken, water is added to adjust the pH value, the mono-ammonium glycyrrhizinate mother liquor paste is dissolved and passes through a resin column 1# to be subjected to chromatography, water elution is carried out to obtain eluent for later use, a resin column 2# is subjected to elution through gradient dilute ethanol, and after the eluent is concentrated and dried under reduced pressure, a liquiritin crude product is obtained; ethanol with the concentration of 95% is added into the crude product, and recrystallization, filtration and drying are carried out to obtain the high-purity liquiritin; (2) the eluent for later use is taken, flows through a resin column 3# and is subjected to water elution, and the eluent is concentrated and dried to obtain the bitterness-removed glycyrrhizin; and (3) the resin columns 1#, 2# and 3# are regeneratedby using the ethanol with the concentration of 95%, eluent is collected and combined, and concentration and drying are carried out to obtain the glycyrrhiza uralensis fisch total flavonoids. Accordingto the production process for jointly separating the high-purity liquiritin, the bitterness-removed glycyrrhizin and the glycyrrhiza uralensis fisch total flavonoids from the mono-ammonium glycyrrhizinate mother liquor paste, the mother liquor paste after production of mono-ammonium glycyrrhizinate is adopted as a raw material, and the three products are separated and purified in a combined mode,so that the comprehensive utilization degree of the raw material is improved, the product value is high, cost is low, reproducibility is good, and the production process is suitable for industrial large-scale production.

Description

technical field [0001] The invention relates to a production process for jointly separating high-purity liquiritin, glycyrrhizic acid and total flavonoids from glycyrrhizic acid monoammonium salt mother liquor paste, belonging to the field of food and medicine. Background technique [0002] Licorice (Glycyrrhiza uralensis Fisch) is a leguminous plant of the genus Glycyrrhiza licorice. There are 29 species and 6 varieties in the world. Among them, there are 3 varieties in 18 in my country, which are widely distributed in Northwest my country, North China, Northeast China and other regions. And Glycyrrhiza glabra is one of the basic plants of the medicinal material Glycyrrhiza glabra, which is widely used in medicine, food, cosmetics and other industries. [0003] The main active ingredients of licorice extract include glycyrrhizic acid and its various analogues of glycyrrhizin saponins, licorice total flavonoids of licorice flavonoids, such as liquiritin, isoliquiritigenin, gl...

Claims

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Application Information

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IPC IPC(8): C07H15/26C07J63/00C07H15/256C07H1/06A61K36/484A61P35/00A61P39/06A61P31/12A61P9/00A61P1/16A61P25/20A61P29/00A61P25/04A23L33/10
CPCC07H15/26C07J63/008C07H15/256C07H1/06A61K36/484A61P35/00A61P39/06A61P31/12A61P9/00A61P1/16A61P25/20A61P29/00A61P25/04A23L33/10A23V2002/00A61K2236/53A23V2200/308A23V2200/30A23V2200/326A23V2200/322A23V2200/32A23V2250/2116
Inventor 高颖霍存录张嘉伟杨恺平张家蓉
Owner 高颖
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