CN110141591A - A kind of saikoside preparation method - Google Patents

A kind of saikoside preparation method Download PDF

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Publication number
CN110141591A
CN110141591A CN201910436279.0A CN201910436279A CN110141591A CN 110141591 A CN110141591 A CN 110141591A CN 201910436279 A CN201910436279 A CN 201910436279A CN 110141591 A CN110141591 A CN 110141591A
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China
Prior art keywords
rhizome
radix bupleuri
saikoside
preparation
saponin
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Pending
Application number
CN201910436279.0A
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Chinese (zh)
Inventor
陈爽
黄硕泉
刘炅峰
段志贵
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Foshan Ou Ruera Biotechnology Co Ltd
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Foshan Ou Ruera Biotechnology Co Ltd
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Priority to CN201910436279.0A priority Critical patent/CN110141591A/en
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A61K36/233—Bupleurum
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation 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
    • A61K2236/10—Preparation or pretreatment of starting material
    • A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation 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
    • A61K2236/30—Extraction of the material
    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation 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
    • A61K2236/30—Extraction of the material
    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation 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
    • A61K2236/30—Extraction of the material
    • A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps

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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)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention discloses a kind of saikoside preparation methods, including radix bupleuri rhizome raw material 10g, 90% ethyl alcohol 120g, compound biological enzyme, low-carbon alcohols and macroporous absorbent resin, step of the present invention is careful, first radix bupleuri rhizome is crushed, destroy its plant fiber structure, and the contact area of itself and enzymolysis liquid can also be increased in enzymatic hydrolysis, accelerate the enzymolysis speed of rhizome interplantation fibres, the cellulase that biological enzyme includes, protease and pectase can digest the cell wall of radix bupleuri rhizome and other biological substances, it has been sufficiently destroyed its protozoa structure, saponin(e is released, then the multiple alcohol extracting carried out can come out the saponin extraction in radix bupleuri rhizome, then it is extracted again with ethyl alcohol, obtained initial material is subjected to second extraction, impurity in it is further separated, the present invention can obtain the soaps of high-purity Glycosides, and the saponin(e arrived in fine impurities content it is few compared with existing saponin content.

Description

A kind of saikoside preparation method
Technical field
The invention discloses a kind of saikoside preparation methods, belong to saponin(e preparation preparation technical field.
Background technique
Saikoside is a kind of drug, is used for cold, fever, fevers and chills alternate, distending pain in the chest and hypochondrium etc., the shelf-life is 2 years.
The existing most purity of saikoside is lower, and preparation is that the impurity of remaining is more, and during extraction It is ignored there are also some impurity, most of saikoside on the market is caused to fail sufficient its effect of performance.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the most purity of existing saikoside is lower, preparation is remaining Impurity is more, and is ignored during extraction there are also some impurity, and most of saikoside on the market is caused to fail Abundance plays its effect, a kind of saikoside preparation method is provided, to solve the above problems.
To achieve the above object, the invention provides the following technical scheme: a kind of saikoside preparation method, including radix bupleuri root Stem raw material 10g, 90% ethyl alcohol 120g, compound biological enzyme, low-carbon alcohols and macroporous absorbent resin, preparation step are as follows:
(1) qualified radix bupleuri rhizome washing will be examined, dried；
(2) the radix bupleuri rhizome slice after washing, dry, crushes, partial size 1-1.5mm；
(3) radix bupleuri rhizome is digested using compound biological enzyme, is filtered, obtain enzymatic hydrolysis material；
(4) material extracting in water will be digested, filtering obtains filter residue, and Aqueous extracts retain；
(5) filter residue is successively used to the low-carbon alcohols of 2-5 times 25-32vol.%, 45-52vol.% and 65-75vol.% It extracts repeatedly, each extraction time is 0.5-2h, and the alcohol extract repeatedly extracted retains, wherein alcohol extracting is extracted using adverse current；
(6) merge Aqueous extracts and multiple alcohol extract, obtain radix bupleuri rhizome extracting solution, cross macroporous absorbent resin adsorption treatment, Eluent is collected, is dried after adsorption bleaching to get radix bupleuri rhizome saponin(e initial material；
(7) initial material is put into pulverizing mill and carries out separating twice, partial size is 50-60 μm；
(8) initial material after micro mist is immersed in 12 times of 90% ethyl alcohol, obtains mixed liquor；
(9) mixed liquor is put into a centrifuge and is centrifuged；
(10) mixed liquor after centrifugation is stood 120 minutes, takes supernatant；
(11) supernatant heating water bath is stopped into heating, Slow cooling, volatilization obtain saponin extract to after 40~50 DEG C.
Preferably, the radix bupleuri rhizome is radix bupleuri scorzoneraefolii rhizome.
Preferably, being ultrasonically treated while the enzymatic hydrolysis, sonication treatment time 1.
Preferably, the material that will digest is using 7-11 times of water extraction 1.5h.
Preferably, the enzymatic hydrolysis material extracts 1h using 10-12 times of water.
Preferably, the low-carbon alcohols are the low-carbon alcohols that carbon atom number is C3.
Preferably, the model of the macroporous absorbent resin be selected from one of HPD-400, D4020 or DS-401 or At least two combination.
Preferably, the compound biological enzyme includes cellulase, protease and pectase.
Compared with prior art, beneficial effects of the present invention are as follows:
Step of the present invention is careful, first crushes radix bupleuri rhizome, destroys its plant fiber structure, and can be in enzymatic hydrolysis Increase its contact area with enzymolysis liquid, accelerates the enzymolysis speed of rhizome interplantation fibres, cellulase that biological enzyme includes, egg White enzyme and pectase can digest the cell wall of radix bupleuri rhizome and other biological substances, be sufficiently destroyed its protozoa structure, Saponin(e is released, the multiple alcohol extracting then carried out can come out the saponin extraction in radix bupleuri rhizome, so It is extracted again with ethyl alcohol afterwards, obtained initial material is subjected to second extraction, the impurity in it is further separated, the present invention can obtain To the saponin(e of high-purity, and the saponin(e arrived in fine impurities content it is few compared with existing saponin content.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects It encloses.
A kind of saikoside preparation method, including radix bupleuri rhizome raw material 10g, 90% ethyl alcohol 120g, compound biological enzyme, low-carbon Pure and mild macroporous absorbent resin, preparation step are as follows:
(1) qualified radix bupleuri rhizome washing will be examined, dried；
(2) the radix bupleuri rhizome slice after washing, dry, crushes, partial size 1-1.5mm；
(3) radix bupleuri rhizome is digested using compound biological enzyme, is filtered, obtain enzymatic hydrolysis material；
(4) material extracting in water will be digested, filtering obtains filter residue, and Aqueous extracts retain；
(5) filter residue is successively used to the low-carbon alcohols of 2-5 times 25-32vol.%, 45-52vol.% and 65-75vol.% It extracts repeatedly, each extraction time is 0.5-2h, and the alcohol extract repeatedly extracted retains, wherein alcohol extracting is extracted using adverse current；
(6) merge Aqueous extracts and multiple alcohol extract, obtain radix bupleuri rhizome extracting solution, cross macroporous absorbent resin adsorption treatment, Eluent is collected, is dried after adsorption bleaching to get radix bupleuri rhizome saponin(e initial material；
(7) initial material is put into pulverizing mill and carries out separating twice, partial size is 50-60 μm；
(8) initial material after micro mist is immersed in 12 times of 90% ethyl alcohol, obtains mixed liquor；
(9) mixed liquor is put into a centrifuge and is centrifuged；
(10) mixed liquor after centrifugation is stood 120 minutes, takes supernatant；
(11) supernatant heating water bath is stopped into heating, Slow cooling, volatilization obtain saponin extract to after 40~50 DEG C.
Wherein, the radix bupleuri rhizome is radix bupleuri scorzoneraefolii rhizome.
Wherein, it is ultrasonically treated while the enzymatic hydrolysis, sonication treatment time 1.
Wherein, the enzymatic hydrolysis material extracts 1.5h using 7-11 times of water.
Wherein, the enzymatic hydrolysis material extracts 1h using 10-12 times of water.
Wherein, the low-carbon alcohols are the low-carbon alcohols that carbon atom number is C3.
Wherein, the model of the macroporous absorbent resin is selected from one of HPD-400, D4020 or DS-401 or at least Two kinds of combination.
Wherein, the compound biological enzyme includes cellulase, protease and pectase.
Specifically, step of the present invention is careful, first radix bupleuri rhizome is crushed, destroys its plant fiber structure, and digesting When can also increase the contact area of itself and enzymolysis liquid, accelerate the enzymolysis speed of rhizome interplantation fibres, the fibre that biological enzyme includes The cell wall of radix bupleuri rhizome and other biological substances can be digested by tieing up plain enzyme, protease and pectase, be sufficiently destroyed its original Biological structure is released saponin(e, and the multiple alcohol extracting then carried out can mention the saponin(e in radix bupleuri rhizome It takes out, is then extracted again with ethyl alcohol, obtained initial material is subjected to second extraction, the impurity in it is further separated, this Invent the saponin(e of available high-purity, and the saponin(e arrived in fine impurities content compared with existing saponin content It is few.
It 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 variations, modification, replacement can be carried out to these embodiments 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 (8)

1. a kind of saikoside preparation method, which is characterized in that including radix bupleuri rhizome raw material 10g, 90% ethyl alcohol 120g, compound life Object enzyme, low-carbon alcohols and macroporous absorbent resin, preparation step are as follows:
(1) qualified radix bupleuri rhizome washing will be examined, dried；
(2) the radix bupleuri rhizome slice after washing, dry, crushes, partial size 1-1.5mm；
(3) radix bupleuri rhizome is digested using compound biological enzyme, is filtered, obtain enzymatic hydrolysis material；
(4) material extracting in water will be digested, filtering obtains filter residue, and Aqueous extracts retain；
(5) filter residue is successively used to the low-carbon alcohol extracting of 2-5 times 25-32vol.%, 45-52vol.% and 65-75vol.% Repeatedly, each extraction time is 0.5-2h, and the alcohol extract repeatedly extracted retains, wherein alcohol extracting is extracted using adverse current；
(6) merge Aqueous extracts and multiple alcohol extract, obtain radix bupleuri rhizome extracting solution, cross macroporous absorbent resin adsorption treatment, collect Eluent is dried to get radix bupleuri rhizome saponin(e initial material after adsorption bleaching；
(7) initial material is put into pulverizing mill and carries out separating twice, partial size is 50-60 μm；
(8) initial material after micro mist is immersed in 12 times of 90% ethyl alcohol, obtains mixed liquor；
(9) mixed liquor is put into a centrifuge and is centrifuged；
(10) mixed liquor after centrifugation is stood 120 minutes, takes supernatant；
(11) supernatant heating water bath is stopped into heating, Slow cooling, volatilization obtain saponin extract to after 40~50 DEG C.
2. a kind of saikoside preparation method according to claim 1, it is characterised in that: the radix bupleuri rhizome is narrow leaf bavin Hu rhizome.
3. a kind of saikoside preparation method according to claim 1, it is characterised in that: surpassed while the enzymatic hydrolysis Sonication, sonication treatment time 1h.
4. a kind of saikoside preparation method according to claim 1, it is characterised in that: the enzymatic hydrolysis material uses 7-11 Water again extracts 1.5h.
5. a kind of saikoside preparation method according to claim 1, it is characterised in that: the enzymatic hydrolysis material uses 10- 12 times of water extracts 1h.
6. a kind of saikoside preparation method according to claim 1, it is characterised in that: the low-carbon alcohols are carbon atom number For the low-carbon alcohols of C3.
7. a kind of saikoside preparation method according to claim 1, it is characterised in that: the type of the macroporous absorbent resin Number combination selected from one of HPD-400, D4020 or DS-401 or at least two.
8. a kind of saikoside preparation method according to claim 1, it is characterised in that: the compound biological enzyme includes fibre Tie up plain enzyme, protease and pectase.
CN201910436279.0A 2019-05-23 2019-05-23 A kind of saikoside preparation method Pending CN110141591A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112546014A (en) * 2020-12-15 2021-03-26 铜仁职业技术学院 Traditional Chinese medicine effervescent tablet for dispelling effects of alcohol and protecting liver and preparation method thereof
CN116019848A (en) * 2023-03-02 2023-04-28 西藏天虹科技股份有限责任公司 Method for extracting saikosaponin from bupleurum

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101322758A (en) * 2008-08-01 2008-12-17 天津商业大学 Method for producing spina date seed extract using complex enzyme
CN102432664A (en) * 2011-12-29 2012-05-02 陕西科技大学 Method for extracting theasaponin from tea seed pulp
CN105769953A (en) * 2016-03-04 2016-07-20 脱德明 Enzymolysis method for extracting medicinal ingredients from bupleurum
CN108743653A (en) * 2018-08-30 2018-11-06 佛山市欧若拉生物科技有限公司 A kind of glycyrrhizin preparation method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101322758A (en) * 2008-08-01 2008-12-17 天津商业大学 Method for producing spina date seed extract using complex enzyme
CN102432664A (en) * 2011-12-29 2012-05-02 陕西科技大学 Method for extracting theasaponin from tea seed pulp
CN105769953A (en) * 2016-03-04 2016-07-20 脱德明 Enzymolysis method for extracting medicinal ingredients from bupleurum
CN108743653A (en) * 2018-08-30 2018-11-06 佛山市欧若拉生物科技有限公司 A kind of glycyrrhizin preparation method

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112546014A (en) * 2020-12-15 2021-03-26 铜仁职业技术学院 Traditional Chinese medicine effervescent tablet for dispelling effects of alcohol and protecting liver and preparation method thereof
CN112546014B (en) * 2020-12-15 2023-01-31 铜仁职业技术学院 Traditional Chinese medicine effervescent tablet for dispelling effects of alcohol and protecting liver and preparation method thereof
CN116019848A (en) * 2023-03-02 2023-04-28 西藏天虹科技股份有限责任公司 Method for extracting saikosaponin from bupleurum

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Application publication date: 20190820