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CN107412319A - A kind of efficiency reduces the method for glycyrrhizic acid and enoxolone in liquorice flavonoids compound - Google Patents

A kind of efficiency reduces the method for glycyrrhizic acid and enoxolone in liquorice flavonoids compound Download PDF

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Publication number
CN107412319A
CN107412319A CN201710409338.6A CN201710409338A CN107412319A CN 107412319 A CN107412319 A CN 107412319A CN 201710409338 A CN201710409338 A CN 201710409338A CN 107412319 A CN107412319 A CN 107412319A
Authority
CN
China
Prior art keywords
enoxolone
resin
filtering
glycyrrhizic acid
efficiency reduces
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710409338.6A
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Chinese (zh)
Inventor
马晓峰
周寒利
苗田清
刘玉良
罗恒磊
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Xinjiang All Taixing Pharmaceutical Technology Co Ltd
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Xinjiang All Taixing Pharmaceutical Technology Co Ltd
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Publication date
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Priority to CN201710409338.6A priority Critical patent/CN107412319A/en
Publication of CN107412319A publication Critical patent/CN107412319A/en
Pending legal-status Critical Current

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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/48Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
    • A61K36/484Glycyrrhiza (licorice)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/55Liquid-liquid separation; Phase separation

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  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Medical Informatics (AREA)
  • Medicinal Chemistry (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention discloses a kind of efficiency to reduce the method for glycyrrhizic acid and enoxolone in liquorice flavonoids compound, and a certain amount of macroporous absorbent resin or ion exchange resin are added in alcohol extract, stirs 5min, stand more than 16h, filtering, filtrate are condensed into medicinal extract, add alkali lye, stand more than 24h, filtering, filtrate add hydrochloric acid regulation pH value to be 5, filtering, it is 7 that filter residue, which is washed to pH value, and filter residue and drying is got product.Present invention reduces content of the glycyrrhetic acid content without reducing active ingredient, product qualification rate is substantially increased, qualification rate is by original 32% to 98%.

Description

A kind of efficiency reduces the method for glycyrrhizic acid and enoxolone in liquorice flavonoids compound
Technical field
Reduced the present invention relates to chemistry, chemical technology field, more particularly to a kind of efficiency sweet in liquorice flavonoids compound The method of oxalic acid and enoxolone.
Background technology
Liquorice flavonoids compound has the effect such as antitumor, anti-inflammatory, anti-oxidant, anti-arrhythmia, liver protection.From radix glycyrrhizae or When liquorice flavonoids compound is extracted in glycyrrhiza extract, part glycyrrhizic acid and enoxolone, glycyrrhizic acid and radix glycyrrhizae are often extracted Hypo acid may cause the side effects such as water-sodium retention after being taken in by human body, therefore glycyrrhizic acid and enoxolone are usually listed in radix glycyrrhizae Limitation in flavone compound medicine checks part.
Macroreticular resin (macroporous resin) is also known as full porous resin, is using styrene and propionic ester as monomer, adds It is crosslinking agent to enter Ethenylbenzene, and toluene, dimethylbenzene are pore-foaming agent, and their polymerizations that are cross-linked with each other form porous skeleton structure.Resin Generally white spherical particle, granularity be 20~60 mesh, is the cross-linked polymer of one kind group containing ion exchange, its physics and chemistry Property is stable, insoluble in acid, alkali and organic solvent, is not influenceed by inorganic salts and strong ion low molecular compound.Resin is inhaled Attached effect is the Van der Waals force for relying on it between adsorbed molecule (adsorbate), passes through its huge ratio surface and carries out thing Reason is adsorbed and worked, and organic compound is reached according to having absorption affinity and its molecular size range to be separated through the elution of certain solvent To different purposes such as separation, purifying, removal of impurities, concentrations.
Ion exchange resin is with functional group's (active group for having exchange ion), has network structure, insoluble High-molecular compound.The species of chemical active radical determines the main character and classification of resin, these active groups in resin It is to exchange functional group, some cations (such as H+ or Na+) or anion (such as OH- or Cl-) can be dissociated in the solution, together When adsorbent solution in other cations or anion for having originally.Ion i.e. in resin mutually intersects with the ion in solution Change, so as to which the ion isolation in solution be come out.
The content of the invention
It is an object of the invention to provide a kind of efficiency to reduce glycyrrhizic acid and enoxolone in liquorice flavonoids compound Method:
A kind of efficiency reduces the method for glycyrrhizic acid and enoxolone in liquorice flavonoids compound, comprises the following steps: A certain amount of macroporous absorbent resin or ion exchange resin are added in alcohol extract, stirs 5min, stands more than 16h, is filtered, filtrate is dense Shorten medicinal extract into, add alkali lye, stand more than 24h, filtering, filtrate adds hydrochloric acid regulation pH value to be 5, and filtering, filter residue is washed to pH value and is 7, filter residue and drying is got product.
Preferably, macroporous absorbent resin or ion exchange resin addition are 10 grams.
Preferably, model ADS-7, ADS-F8 or LX-16 of the macroporous absorbent resin.
The beneficial effects of the invention are as follows:Content present invention reduces glycyrrhetic acid content without reduction active ingredient, greatly Product qualification rate is improved greatly, qualification rate is by original 32% to 98%.
Embodiment
The technical scheme in the embodiment of the present invention is clearly and completely described below, it is clear that described embodiment Only part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, the common skill in this area The every other embodiment that art personnel are obtained under the premise of creative work is not made, belong to the model that the present invention protects Enclose.
A kind of efficiency reduces the method for glycyrrhizic acid and enoxolone in liquorice flavonoids compound, comprises the following steps:
A certain amount of macroporous absorbent resin or ion exchange resin are added in alcohol extract, stirs 5min, stands more than 16h, Filtering, filtrate are condensed into medicinal extract, add alkali lye, stand more than 24h, filtering, and filtrate adds hydrochloric acid regulation pH value to be 5, filtering, filter residue water It is 7 to be washed till pH value, and filter residue and drying is got product.Content present invention reduces glycyrrhetic acid content without reduction active ingredient, Product qualification rate is substantially increased, qualification rate is by original 32% to 98%.
8 kind (1 is added in alcohol extract by the above method:XDA-1、2:ADS-7、3:ADS-F8、4:XDA-8、5:LX- 16、6:LX-162、7:LX-T19、8:LX-201) resin of different model is numbered by natural number respectively, and 1-6 resins are macropore Polymeric adsorbent, 7-8 resins are ion exchange resin, and resin amount is 10g, the final products through 1-8 resin treatments Enoxolone reduces by 14.7%, 38.0%, 30.1%, 59.2%, 51.6%, 17.8%, 69.3%, 80.0% respectively, but produces Product active ingredient reduces by 38.5%, 22.9%, 23.2%, 62.8%, 39.5%, 19.7%, 64.8%, 80.1 respectively, synthesis Consider that choosing enoxolone reduces the resin that amplitude is more than active ingredient attenuating amplitude, therefore preferably No. 2, No. 3, No. 5 resin types Number it is optimal.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding And modification, the scope of the present invention is defined by the appended.

Claims (3)

1. a kind of efficiency reduces the method for glycyrrhizic acid and enoxolone in liquorice flavonoids compound, it is characterised in that including such as Lower step:A certain amount of macroporous absorbent resin or ion exchange resin are added in alcohol extract, stirs 5min, stands more than 16h, mistake Filter, filtrate are condensed into medicinal extract, add alkali lye, stand more than 24h, filtering, and filtrate adds hydrochloric acid regulation pH value to be 5, filtering, filter residue washing It is 7 to pH value, filter residue and drying is got product.
2. a kind of efficiency reduces the method for glycyrrhizic acid and enoxolone in liquorice flavonoids compound, it is characterised in that macropore is inhaled Attached resin or ion exchange resin addition is 10 grams.
3. a kind of efficiency reduces the method for glycyrrhizic acid and enoxolone in liquorice flavonoids compound, it is characterised in that described big Model ADS-7, ADS-F8 or LX-16 of macroporous adsorbent resin.
CN201710409338.6A 2017-06-02 2017-06-02 A kind of efficiency reduces the method for glycyrrhizic acid and enoxolone in liquorice flavonoids compound Pending CN107412319A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710409338.6A CN107412319A (en) 2017-06-02 2017-06-02 A kind of efficiency reduces the method for glycyrrhizic acid and enoxolone in liquorice flavonoids compound

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710409338.6A CN107412319A (en) 2017-06-02 2017-06-02 A kind of efficiency reduces the method for glycyrrhizic acid and enoxolone in liquorice flavonoids compound

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CN107412319A true CN107412319A (en) 2017-12-01

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108114018A (en) * 2018-01-18 2018-06-05 新疆乌拉尔甘草开发有限责任公司 A kind of method for preparing alcohol-soluble licoflavone
CN113105423A (en) * 2021-03-05 2021-07-13 新疆全安药业股份有限公司 Method for extracting licoflavone by controlling glycyrrhizic acid content

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1563073A (en) * 2004-04-06 2005-01-12 南开大学 Method for preparing enoxolone
CN101747307A (en) * 2009-12-22 2010-06-23 江苏天晟药业有限公司 Glycyrrhizic acid removal glycyrrhiza flavonoid and medicament composition thereof
CN102453075A (en) * 2010-10-26 2012-05-16 曾科 Separation and purification process of glycyrrhizic acid
CN102836202A (en) * 2012-09-18 2012-12-26 波拉提·马卡比力 A method for comprehensive development and utilization of aboveground parts of licorice
CN106619798A (en) * 2016-12-27 2017-05-10 新疆全泰兴药业科技有限公司 Extracting process of licorice flavonoid compound

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1563073A (en) * 2004-04-06 2005-01-12 南开大学 Method for preparing enoxolone
CN101747307A (en) * 2009-12-22 2010-06-23 江苏天晟药业有限公司 Glycyrrhizic acid removal glycyrrhiza flavonoid and medicament composition thereof
CN102453075A (en) * 2010-10-26 2012-05-16 曾科 Separation and purification process of glycyrrhizic acid
CN102836202A (en) * 2012-09-18 2012-12-26 波拉提·马卡比力 A method for comprehensive development and utilization of aboveground parts of licorice
CN106619798A (en) * 2016-12-27 2017-05-10 新疆全泰兴药业科技有限公司 Extracting process of licorice flavonoid compound

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
王巧娥等: "《甘草深加工技术》", 31 January 2011, 中国轻工业出版社 *
第7期: "基于熵权法的多目标筛选甘草黄酮类成分纯化工艺", 《中草药》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108114018A (en) * 2018-01-18 2018-06-05 新疆乌拉尔甘草开发有限责任公司 A kind of method for preparing alcohol-soluble licoflavone
CN113105423A (en) * 2021-03-05 2021-07-13 新疆全安药业股份有限公司 Method for extracting licoflavone by controlling glycyrrhizic acid content

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Application publication date: 20171201