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Production process for combined separation of various licorice active components

An active ingredient and production process technology, which is applied in the production process field of joint separation of multiple licorice active ingredients, can solve the problems of difficult operation, cumbersome operation, classification and collection, etc., so as to avoid organic solvent residues, high resource utilization, and reduce The effect of security risks

Pending Publication Date: 2021-11-19
GANSU YALAN PHARMA
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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
[0008] 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.
[0009] Gansu Fanzhi Pharmaceutical Co., Ltd. has applied for a technology called "A process for the joint separation of high-purity liquiritin, debittering glycyrrhizin and total flavonoids of licorice from glycyrrhizinate monoammonium salt mother liquid paste" (application number: 202011128456.8 ), the patent eluted glycyrrhizinate monoammonium salt mother liquor paste with different types of resins to obtain liquiritin, and co-produced three products of glycyrrhizin and licorice flavonoids at the same time. Although the raw materials can be fully and effectively utilized, However, the flavonoid components such as liquiritigenin and isoliquiritigenin coexisting with liquiritin have not been classified and collected, and the elution solvent consumption of macroporous resin is large, and the operation is cumbersome and inconvenient for large-scale production
[0010] 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

[0037] Embodiment 1 A kind of production technique of joint separation multiple active ingredients of licorice, comprises the following steps:

[0038] (1) In the jacketed pot, add 10 kg of mother liquor powder produced after the production of monoammonium glycyrrhizinate, add 50 L of ethyl acetate each time, stir and extract at room temperature for 3 times, and obtain the extract and ethyl acetate insolubles respectively.

[0039] (2) The extract is filtered, recovered and dissolved, dried and pulverized to obtain 3.5kg of product A; put the product A into a jacketed pot, add 12L of purified water each time, heat and stir at 100°C for 3 times, and extract for 1-2 hours each time. After stirring and extracting, it was allowed to stand for precipitation to obtain supernatant and product B respectively. Product B is the water insoluble fraction.

[0040] The supernatant was concentrated under reduced pressure to 2.5kg of clear cream with a specific gravity of 1.15 (60°C), and 5...

Embodiment 2

[0043] Embodiment 2 A kind of production technology of joint separation multiple active ingredients of licorice, comprises the following steps:

[0044] (1) In the jacketed pot, add 10 kg of mother liquor powder produced after the production of monoammonium glycyrrhizinate, add 30 L of ethyl acetate each time, stir and extract at room temperature for 3 times, and obtain the extract and ethyl acetate insolubles respectively.

[0045] (2) The extract is filtered, recovered, dissolved, dried, and pulverized to obtain 2.8kg of product A; add product A to a jacketed pot, add 0.4L of purified water each time, heat and stir at 60°C for 3 times, and extract for 1-2 hours each time . After stirring and extracting, it was allowed to stand for precipitation to obtain supernatant and product B respectively. Product B is the water insoluble fraction.

[0046] Concentrate the supernatant under reduced pressure to 2kg of clear paste with a specific gravity of 1.20 (60°C), add 3BV of ethano...

Embodiment 3

[0049] Embodiment 3 A kind of production technology of joint separation multiple active ingredients of licorice, comprises the following steps:

[0050] (1) In the jacketed pot, add 10kg of mother liquor powder after producing monoammonium glycyrrhizinate, add 40L of ethyl acetate each time, stir and extract twice at room temperature, and obtain extract and ethyl acetate insoluble matter respectively.

[0051] (2) The extract is filtered, recovered and dissolved, dried and pulverized to obtain 2.2kg of product A; add product A to the jacketed pot, add 8.8L of purified water each time, heat and stir at 40°C for 1 time, and extract 1~2 hours each time . After stirring and extracting, it was allowed to stand for precipitation to obtain supernatant and product B respectively. Product B is the water insoluble fraction.

[0052] The supernatant was concentrated under reduced pressure to 1.5kg of a clear paste with a specific gravity of 1.18 (60°C), added 1L of ethanol with a volum...

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PUM

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Abstract

The invention relates to a production process for combined separation of a plurality of licorice active components, which comprises the following steps: (1) stirring and extracting mother liquor powder and a solvent after production of mono-ammonium glycyrrhizinate at room temperature to obtain an extracting solution and a solvent insoluble part; (2) filtering, recovering, dissolving, drying and crushing the extracting solution to obtain a product A; adding purified water into the product A, heating, stirring and extracting to obtain supernate and a product B; concentrating the supernate under reduced pressure, adding 95% ethanol, and heating to dissolve the supernate; and sequentially adding activated carbon for decoloration, filtering, standing for crystallization, separating and recrystallizing to obtain liquiritin with the content of more than 90%, (3) performing vacuum drying and normal-pressure heating on the insoluble part of the solvent to obtain a product C, and drying and crushing the product C to obtain the debittered glycyrrhizin with the glycyrrhizic acid content of more than 10%; and (4) carrying out vacuum drying and crushing on the product B to obtain crude liquiritigenin and isoliquiritigenin with the content of 8-15%. The method is simple in process, low in cost, high in safety and suitable for industrial large-scale production.

Description

technical field [0001] The invention relates to the fields of food and medicine, in particular to a production process for combining and isolating multiple active components of licorice. Background technique [0002] Licorice (Glycyrrhiza uralensis Fisch) is a leguminous licorice plant. There are 29 species and 6 varieties in the world. Among them, there are 18 species and 3 varieties in my country. They are widely distributed in Northwest China, 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 analogs of glycyrrhizin saponins, licorice total flavonoids of licorice flavonoids, such as liquiritin, glycyrrhizin, isoliquiritigenin, glabridin, etc., and licorice polysaccharides. [0004] Among them, Liquiritin (Liquir...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/26C07H1/06C07D311/32C07D311/40C07C45/78C07C45/81C07C49/835C07J63/00
CPCC07H15/26C07H1/06C07D311/32C07D311/40C07C45/78C07C45/81C07J63/008C07C49/835
Inventor 张继义罗兴平张丹
Owner GANSU YALAN PHARMA
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