CN110156862A - A kind of method that separation prepares antineoplastic component ganoderic acid - Google Patents

A kind of method that separation prepares antineoplastic component ganoderic acid Download PDF

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Publication number
CN110156862A
CN110156862A CN201910215193.5A CN201910215193A CN110156862A CN 110156862 A CN110156862 A CN 110156862A CN 201910215193 A CN201910215193 A CN 201910215193A CN 110156862 A CN110156862 A CN 110156862A
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China
Prior art keywords
ganoderic acid
beaker
glossy ganoderma
ganoderma powder
paper bag
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CN201910215193.5A
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Chinese (zh)
Inventor
刘月芹
贺晓龙
高小朋
任佳梅
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Yanan University
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Yanan University
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Priority to CN201910215193.5A priority Critical patent/CN110156862A/en
Publication of CN110156862A publication Critical patent/CN110156862A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07JSTEROIDS
    • C07J9/00Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of more than two carbon atoms, e.g. cholane, cholestane, coprostane
    • C07J9/005Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of more than two carbon atoms, e.g. cholane, cholestane, coprostane containing a carboxylic function directly attached or attached by a chain containing only carbon atoms to the cyclopenta[a]hydrophenanthrene skeleton

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention discloses a kind of methods that separation prepares antineoplastic component ganoderic acid, include the following steps: step 1: clean, dustless ganoderma lucidum fruitbody being taken to be crushed;Step 2: taking aperture is that the mesh screen of 0.25mm screens the glossy ganoderma powder after grinding;Step 3: the tin paper bag for holding glossy ganoderma powder is rolled, and the glossy ganoderma powder on tin paper bag is poured into beaker, while the ethanol solution that concentration is 85% is poured into beaker, is then stirred using blender to the solution in beaker;Step 4: beaker is heated by alcolhol burner;Step 5: gained crystal in step 4 is filtered collection, and gained concentrate in step 4 is added the concussion of petroleum ether extraction 3 to 5 times;Step 6: high-speed countercurrent chromatography separates ganoderic acid.When preparing ganoderic acid, the preparation efficiency and preparation effect of ganoderic acid are effectively increased;Reduce the cost for preparing ganoderic acid.

Description

A kind of method that separation prepares antineoplastic component ganoderic acid
Technical field
The present invention relates to a kind of pharmaceutical technology, method that specifically a kind of separation prepares antineoplastic component ganoderic acid.
Background technique
The content of ganoderic acid is the raising with its maturity and is incremented by ganoderma lucidum fruitbody, and concentrates on the outer of fructification All positions.Ganoderic acid is mostly tetracyclic triterpene, is highly oxidized lanostane.Ganoderic acid can inhibit releasing for cell tissue amine It puts, the function of the various organs of digestive system can be enhanced, also there is reducing blood lipid, blood pressure lowering, protect liver, adjust river note ganoderma lucidum row ganoderma lucidum The effects of ganoderma lucidum row lucidum spore powder liver function, is remembered in conidia powder river, is a kind of with multiple effects such as analgesic, calmness, anticancer, removing toxic substances The natural organic-compound of energy.Ganoderic acid why can reducing blood lipid, blood pressure lowering, be because ganoderic acid block lanosterol or The ability of dioxy lanosterol synthetic cholesterol, and then slow down atherosclerosis, slow down the process that blood pressure increases.Since clever Sesame acid has above-mentioned positive effectiveness, therefore the content of ganoderic acid becomes as one of ganoderma lucidum and its important indicator of product.And show Some technological means are at high cost when preparing ganoderic acid, and concentration is low, are not suitable for the ganoderic acid preparation of high-purity.
Summary of the invention
The purpose of the present invention is to provide a kind of methods that separation prepares antineoplastic component ganoderic acid, to solve above-mentioned background The problem of being proposed in technology.
To achieve the above object, the invention provides the following technical scheme:
A kind of method that separation prepares antineoplastic component ganoderic acid, includes the following steps:
Step 1: clean, dustless ganoderma lucidum fruitbody 1000g is taken, is crushed;
Step 2: taking aperture is that the mesh screen of 0.25mm screens the glossy ganoderma powder after grinding, and ganoderma powder is placed into In mesh screen, and mesh screen is manually made to carry out annular vibration in the horizontal direction, sieves the glossy ganoderma powder fallen and held with tin paper bag;
Step 3: the tin paper bag for holding glossy ganoderma powder is rolled, and the glossy ganoderma powder on tin paper bag is poured into beaker, while to The ethanol solution that concentration is 85% is poured into beaker, and then the solution in beaker is stirred using blender;
Step 4: heating beaker by alcolhol burner, when the temperature in beaker is heated to alcohol boiling, thus to step Obtained solution is concentrated in rapid three, and heating time is set to 1-2 hours;
Step 5: gained crystal in step 4 is filtered collection, and gained concentrate in step 4 is added 1-5 times The concussion of petroleum ether extraction 3 to 5 times, 2-5 hours are stood every time, petroleum ether extraction liquid is concentrated under reduced pressure, to obtain spirit The extract of sesame acid;
Step 6: high-speed countercurrent chromatography separates ganoderic acid: solvent is made of n-hexane, ethyl acetate, first alcohol and water, is pressed It is mixed according to 4-5: 4-5: 2-3: 6-8 volume ratio, phase is taken to make stationary phase, lower phase is mobile phase, and extract mixes under Simultaneously sample introduction is solved, high speed adverse current chromatogram range of speeds 750-900r/min, flow rates 1-3ml/min, every 5-8ml are collected as one Then a fraction detects the ingredient of each test tube collection liquid with high-efficient liquid phase chromatogram technique analysis, then collect by heterogeneity, is dense It contracts, is dry, isolated ganoderic acid.
As a further solution of the present invention: herb roller carries out fine gtinding to ganoderma lucidum fruitbody in using when crushing, will Ganoderma lucidum fruitbody is pulverized.
As a further solution of the present invention: the mixing time of blender is 15min.
As a further solution of the present invention: the volume of ethanol solution is 5-10 times of glossy ganoderma powder.
Compared with prior art, inverse by evaporative crystallization and high speed the beneficial effects of the present invention are: when preparing ganoderic acid Flow chromatography separates ganoderic acid, the ganoderma lucidum acid product of high-purity can be obtained, to effectively increase the preparation efficiency of ganoderic acid With preparation effect;Used material is usual equipment when preparing ganoderic acid, and equipment is common to be easy to get, to reduce preparation The cost of ganoderic acid.
Specific embodiment
Below in conjunction in the embodiment of the present invention, technical solution in the embodiment of the present invention is clearly and completely retouched It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention In embodiment, every other implementation obtained by those of ordinary skill in the art without making creative efforts Example, shall fall within the protection scope of the present invention.
In the embodiment of the present invention, a kind of method that separation prepares antineoplastic component ganoderic acid, the specific steps of which are as follows:
Step 1: taking clean, dustless ganoderma lucidum fruitbody 1000g, crushed, when crushing use in herb roller carry out essence Ganoderma lucidum fruitbody is pulverized in fine lapping;
Step 2: taking aperture is that the mesh screen of 0.25mm screens the glossy ganoderma powder after grinding, and ganoderma powder is placed into In mesh screen, and mesh screen is manually made to carry out annular vibration in the horizontal direction, so that fine ganoderma powder be sieved, sieve is fallen Glossy ganoderma powder held with tin paper bag;
Step 3: the tin paper bag for holding glossy ganoderma powder is rolled, and the glossy ganoderma powder on tin paper bag is poured into beaker, while to The ethanol solution that concentration is 85% is poured into beaker, the volume of ethanol solution is 5-10 times of glossy ganoderma powder, then uses blender Solution in beaker is stirred, mixing time 15min;
Step 4: heating beaker by alcolhol burner, when the temperature in beaker is heated to alcohol boiling, thus to step Obtained solution is concentrated in rapid three, and heating time is set to 1-2 hours, so that ganoderic acid be made to be precipitated from solution, is become Crystal obtains the concentrate of ganoderma lucidum acid crystal and ganoderic acid ethanol solution;
Step 5: gained crystal in step 4 is filtered collection, and gained concentrate in step 4 is added 1-5 times The concussion of petroleum ether extraction 3 to 5 times, 2-5 hours are stood every time, petroleum ether extraction liquid is concentrated under reduced pressure, to obtain spirit The extract of sesame acid;
Step 6: high-speed countercurrent chromatography separates ganoderic acid: solvent is made of n-hexane, ethyl acetate, first alcohol and water, is pressed It is mixed according to 4-5: 4-5: 2-3: 6-8 volume ratio, phase is taken to make stationary phase, lower phase is mobile phase, and extract mixes under Simultaneously sample introduction is solved, high speed adverse current chromatogram range of speeds 750-900r/min, flow rates 1-3ml/min, every 5-8ml are collected as one Then a fraction detects the ingredient of each test tube collection liquid with high-efficient liquid phase chromatogram technique analysis, then collect by heterogeneity, is dense It contracts, is dry, isolated ganoderic acid.
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, It is still possible to modify the technical solutions described in the foregoing embodiments, or carries out to part of technical characteristic Equivalent replacement, all within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should all include Within protection scope of the present invention.

Claims (4)

1. a kind of method that separation prepares antineoplastic component ganoderic acid, which comprises the steps of:
Step 1: clean, dustless ganoderma lucidum fruitbody 1000g is taken, is crushed;
Step 2: taking aperture is that the mesh screen of 0.25mm screens the glossy ganoderma powder after grinding, and ganoderma powder is placed into mesh screen In, and mesh screen is manually made to carry out annular vibration in the horizontal direction, it sieves the glossy ganoderma powder fallen and is held with tin paper bag;
Step 3: the tin paper bag for holding glossy ganoderma powder is rolled, and the glossy ganoderma powder on tin paper bag is poured into beaker, while to beaker In pour into concentration be 85% ethanol solution, then the solution in beaker is stirred using blender;
Step 4: heating beaker by alcolhol burner, when the temperature in beaker is heated to alcohol boiling, thus to step 3 In obtained solution be concentrated, heating time is set to 1-2 hours;
Step 5: gained crystal in step 4 is filtered collection, and 1-5 times of petroleum is added in gained concentrate in step 4 Ether concussion extraction 3 to 5 times, 2-5 hours are stood every time, petroleum ether extraction liquid is concentrated under reduced pressure, to obtain ganoderic acid Extract;
Step 6: high-speed countercurrent chromatography separates ganoderic acid: solvent is made of n-hexane, ethyl acetate, first alcohol and water, according to 4- 5: 4-5: 2-3: 6-8 volume ratio is mixed, and phase is taken to make stationary phase, and lower phase is mobile phase, extract with lower phased soln simultaneously Sample introduction, high speed adverse current chromatogram range of speeds 750-900r/min, flow rates 1-3ml/min, every 5-8ml are collected as one and evaporate Point, the ingredient of each test tube collection liquid is then detected with high-efficient liquid phase chromatogram technique analysis, is then collected, concentration, is done by heterogeneity Dry, isolated ganoderic acid.
2. the method that a kind of separation according to claim 1 prepares antineoplastic component ganoderic acid, which is characterized in that when crushing Herb roller carries out fine gtinding to ganoderma lucidum fruitbody in, and ganoderma lucidum fruitbody is pulverized.
3. the method that a kind of separation according to claim 1 prepares antineoplastic component ganoderic acid, which is characterized in that blender Mixing time be 15min.
4. the method that a kind of separation according to claim 1 prepares antineoplastic component ganoderic acid, which is characterized in that ethyl alcohol is molten The volume of liquid is 5-10 times of glossy ganoderma powder.
CN201910215193.5A 2019-03-14 2019-03-14 A kind of method that separation prepares antineoplastic component ganoderic acid Pending CN110156862A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1998013512A1 (en) * 1996-09-28 1998-04-02 Essential Nutrition Ltd. A method for producing an extract from ganoderma lucidum containing ganoderic acid
CN101559083A (en) * 2009-05-25 2009-10-21 江苏省中医药研究院 Fruiting body extract of Ganoderma Lucidum with antitumor activity and preparation method
CN103724389A (en) * 2013-12-23 2014-04-16 福建仙芝楼生物科技有限公司 Method for separating and preparing anti-tumor components ganoderic acid C1 and ganoderic acid F
CN104725455A (en) * 2015-03-25 2015-06-24 上海市农业科学院 Preparation method of ganoderic acid T

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1998013512A1 (en) * 1996-09-28 1998-04-02 Essential Nutrition Ltd. A method for producing an extract from ganoderma lucidum containing ganoderic acid
CN101559083A (en) * 2009-05-25 2009-10-21 江苏省中医药研究院 Fruiting body extract of Ganoderma Lucidum with antitumor activity and preparation method
CN103724389A (en) * 2013-12-23 2014-04-16 福建仙芝楼生物科技有限公司 Method for separating and preparing anti-tumor components ganoderic acid C1 and ganoderic acid F
CN104725455A (en) * 2015-03-25 2015-06-24 上海市农业科学院 Preparation method of ganoderic acid T

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Application publication date: 20190823