CN108610435A - A kind of ganoderma spore polysaccharide extraction process - Google Patents

A kind of ganoderma spore polysaccharide extraction process Download PDF

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Publication number
CN108610435A
CN108610435A CN201810839542.6A CN201810839542A CN108610435A CN 108610435 A CN108610435 A CN 108610435A CN 201810839542 A CN201810839542 A CN 201810839542A CN 108610435 A CN108610435 A CN 108610435A
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China
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extraction
ganoderma
concentration
butanol
broken wall
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CN201810839542.6A
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Inventor
孟凡欣
吴丽艳
赵成国
杨东生
赵明智
金元宝
王立英
王艳珍
秦书芝
王兰英
耿璐璐
刘雨萌
钟恬
胡玲
李晶莹
张瑶
刘明石
姚易
冯微
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Zhuhai College of Jilin University
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Zhuhai College of Jilin University
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0003General processes for their isolation or fractionation, e.g. purification or extraction from biomass

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Molecular Biology (AREA)
  • General Health & Medical Sciences (AREA)
  • Sustainable Development (AREA)
  • Biochemistry (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)

Abstract

The invention discloses a kind of ganoderma spore polysaccharide extraction processes, include the following steps:Reishi sporule is cleaned after draining, slice, after carrying out secondary low temperature broken wall, it is placed in flash extracter, after 2~3h of alcohol solution dipping that volumetric concentration is 75~85% is added into lucidum spore powder in proportion, after 30~60S being handled at 30~50 DEG C, filtering, then the ethanol solution that volumetric concentration is 75~85% is added into filter residue in proportion, 1~2h of ultrasound at 60 DEG C, filtering, merging filtrate, concentration and recovery ethyl alcohol, the extracting solution of gained is pumped into extraction tower, n-butanol is uniformly introduced in extraction tower in proportion and carries out cycle high-speed counter-current extraction, it is 40~60 DEG C to control extraction temperature, after cycling extraction 3~5 times, concentration and recovery n-butanol, vacuum freeze drying, obtain ganoderma spore polysaccharide.Present invention process is simple, easily operated, and product purity is higher and stable quality.

Description

A kind of ganoderma spore polysaccharide extraction process
Technical field
The invention belongs to natural product chemistry technical field more particularly to a kind of ganoderma spore polysaccharide extraction processes.
Background technology
Ganoderma lucidum polysaccharide is the active ingredient of ganoderma lucidum " strengthening the body resistance to consolidate the constitution ".Ganoderma lucidum polysaccharide is present in ganoderma lucidum mycelium, fructification, spore In the zymotic fluid of sub- powder and ganoderma lucidum engineered strain, the mixture that is made of peptide polysaccharide, glucan, heteroglycan etc..It is big in glucan Part is 2 glucans of β, and minority is 2 glucans of α, and 2 glucans of β are its active main components of performance.Studies have shown that ganoderma lucidum Polysaccharide has extensive physiological activity, with raising immunity of organisms, inhibition tumour, enhancing body's hypoxia tolerance, eliminates certainly The effects that by base, anti-aging.Currently, the method for extraction ganoderma lucidum polysaccharide mostly uses greatly water extraction and alcohol precipitation method, extraction, enzyme process and carries It takes, supercritical fluid assisted extraction and ultrasonic microwave extraction method etc..The ganoderma lucidum polysaccharide extracted with these methods, structure, Bioactivity can be influenced by conditions such as solvent, Extracting temperature, acid-base values and be declined, and there is also recovery rates for these methods not Height, the shortcoming such as impurity is more.
Invention content
It is simple for process, efficient, extract is pure the purpose of the present invention is to provide a kind of ganoderma spore polysaccharide extraction process Degree is high and product quality is stablized.
To achieve the above object, the technical solution that the present invention takes is:
A kind of ganoderma spore polysaccharide extraction process, includes the following steps:
S1, by Reishi sporule clean drain after, slice, be placed in low temperature wall-breaking machine, in -25~10 DEG C, CO2Gas shield Under carry out freezing broken wall, obtain the lucidum spore powder of a broken wall;
S2, under the conditions of the lucidum spore powder of a broken wall is placed in -18 DEG C, after freezing embrittlement 3~5h, in 30~40 DEG C of items Under part, supersonic wave wall breaking processing is carried out, the lucidum spore powder of secondary broken wall is obtained;
S3, the lucidum spore powder of the secondary broken wall of gained is placed in flash extracter, according to 1g:The ratio of 10~30mL After 2~3h of alcohol solution dipping that volumetric concentration is 75~85% is added into lucidum spore powder, 30 are handled at 30~50 DEG C After~60S, filtering obtains filtrate and filter residue;
Then according to 1g:The ethanol solution that volumetric concentration is 75~85% is added into filter residue for the ratio of 10~20mL, in 1~2h of ultrasound at 60 DEG C, filtering, merging filtrate, concentration and recovery ethyl alcohol obtain extracting solution;
S4, the extracting solution of gained is pumped into extraction tower, it is 1 then to press extracting solution with n-butanol volume ratio:1~3 ratio Example uniformly introduces n-butanol in extraction tower and carries out cycle high-speed counter-current extraction, and control extraction temperature is 40~60 DEG C, cycle extraction After taking 3~5 times, extract liquor, concentration and recovery n-butanol are obtained, vacuum freeze drying obtains ganoderma spore polysaccharide.
Further, Reishi sporule is cut into the thin slice that thickness is 0.5mm in the step S1.
Further, the condition of ultrasonication is in the step S2:Supersonic frequency is 18~24 kHz, time 4 ~16min, rotating speed are 20~50rpm.
Further, supersonic frequency is 120~180Hz in the step S3.
The invention has the advantages that:
Present invention process is simple, easily operated, and product purity is higher and stable quality.
Specific implementation mode
In order to make objects and advantages of the present invention be more clearly understood, the present invention is carried out with reference to embodiments further It is described in detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to limit this hair It is bright.
Embodiment 1
A kind of ganoderma spore polysaccharide extraction process, includes the following steps:
S1, by Reishi sporule clean drain after, be cut into thickness be 0.5mm thin slice, be placed in low temperature wall-breaking machine, -25 ℃、CO2Freezing broken wall is carried out under gas shield, obtains the lucidum spore powder of a broken wall;
S2, under the conditions of the lucidum spore powder of a broken wall is placed in -18 DEG C, after freezing embrittlement 3h, under the conditions of 30 DEG C, Supersonic frequency is 18 kHz, and supersonic wave wall breaking handles 16min under conditions of rotating speed is 20rpm, obtains the ganoderma lucidum of secondary broken wall Conidia powder;
S3, the lucidum spore powder of the secondary broken wall of gained is placed in flash extracter, according to 1g:The ratio of 10~30mL After the alcohol solution dipping 3h that volumetric concentration is 75% is added into lucidum spore powder, after handling 30S at 30 DEG C, filtering obtains Filtrate and filter residue;
Then according to 1g:The ethanol solution that volumetric concentration is 75% is added into filter residue for the ratio of 10~20mL, in 60 DEG C Lower supersonic frequency is ultrasound 2h under conditions of 120Hz, is filtered, and merging filtrate, concentration and recovery ethyl alcohol obtains extracting solution;
S4, the extracting solution of gained is pumped into extraction tower, it is 1 then to press extracting solution with n-butanol volume ratio:1 ratio is past N-butanol is uniformly introduced in extraction tower carries out cycle high-speed counter-current extraction, control extraction temperature is 40 DEG C, after cycling extraction 5 times, Extract liquor, concentration and recovery n-butanol are obtained, vacuum freeze drying obtains ganoderma spore polysaccharide.
Embodiment 2
A kind of ganoderma spore polysaccharide extraction process, includes the following steps:
S1, by Reishi sporule clean drain after, be cut into thickness be 0.5mm thin slice, be placed in low temperature wall-breaking machine ,- 17.5℃、CO2Freezing broken wall is carried out under gas shield, obtains the lucidum spore powder of a broken wall;
S2, under the conditions of the lucidum spore powder of a broken wall is placed in -18 DEG C, after freezing embrittlement 4h, under the conditions of 35 DEG C, Supersonic frequency is 21 kHz, and supersonic wave wall breaking handles 10min under conditions of rotating speed is 35rpm, obtains the ganoderma lucidum of secondary broken wall Conidia powder;
S3, the lucidum spore powder of the secondary broken wall of gained is placed in flash extracter, according to 1g:The ratio of 10~30mL After the alcohol solution dipping 2.5h that volumetric concentration is 80% is added into lucidum spore powder, after handling 45S at 40 DEG C, filtering, Obtain filtrate and filter residue;
Then according to 1g:The ethanol solution that volumetric concentration is 80% is added into filter residue for the ratio of 10~20mL, in 60 DEG C Lower supersonic frequency is ultrasound 1.5h under conditions of 150Hz, is filtered, and merging filtrate, concentration and recovery ethyl alcohol obtains extracting solution;
S4, the extracting solution of gained is pumped into extraction tower, it is 1 then to press extracting solution with n-butanol volume ratio:1~3 ratio Example uniformly introduces n-butanol in extraction tower and carries out cycle high-speed counter-current extraction, and control extraction temperature is 50 DEG C, cycling extraction 4 times Afterwards, extract liquor, concentration and recovery n-butanol are obtained, vacuum freeze drying obtains ganoderma spore polysaccharide.
Embodiment 3
A kind of ganoderma spore polysaccharide extraction process, includes the following steps:
S1, by Reishi sporule clean drain after, be cut into thickness be 0.5mm thin slice, be placed in low temperature wall-breaking machine, 5 DEG C, CO2Freezing broken wall is carried out under gas shield, obtains the lucidum spore powder of a broken wall;
S2, under the conditions of the lucidum spore powder of a broken wall is placed in -18 DEG C, after freezing embrittlement 5h, under the conditions of 40 DEG C, Supersonic frequency is 24 kHz, and supersonic wave wall breaking handles 4min under conditions of rotating speed is 50rpm, obtains the ganoderma lucidum spore of secondary broken wall Sub- powder;
S3, the lucidum spore powder of the secondary broken wall of gained is placed in flash extracter, according to 1g:The ratio of 10~30mL After the alcohol solution dipping 2h that volumetric concentration is 85% is added into lucidum spore powder, after handling 60S at 50 DEG C, filtering obtains Filtrate and filter residue;
Then according to 1g:The ethanol solution that volumetric concentration is 85% is added into filter residue for the ratio of 10~20mL, in 60 DEG C Lower supersonic frequency is ultrasound 1h under conditions of 180Hz, is filtered, and merging filtrate, concentration and recovery ethyl alcohol obtains extracting solution;
S4, the extracting solution of gained is pumped into extraction tower, it is 1 then to press extracting solution with n-butanol volume ratio:3 ratio is past N-butanol is uniformly introduced in extraction tower carries out cycle high-speed counter-current extraction, control extraction temperature is 60 DEG C, after cycling extraction 3 times, Extract liquor, concentration and recovery n-butanol are obtained, vacuum freeze drying obtains ganoderma spore polysaccharide.
The ganoderma spove powder polysaccharide that Examples 1 to 3 is prepared is measured respectively, obtains following result:It is real Apply example 1:Polyoses content 56.9%, polysaccharide yield 8.8%;Embodiment 2:Polyoses content 62.1%, polysaccharide yield 10.71%;It is real Apply example 3:Polyoses content 58.9%, polysaccharide yield 7.89%.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, without departing from the principle of the present invention, it can also make several improvements and retouch, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims (4)

1. a kind of ganoderma spore polysaccharide extraction process, it is characterised in that:Include the following steps:
S1, by Reishi sporule clean drain after, slice, be placed in low temperature wall-breaking machine, in -25~10 DEG C, CO2Under gas shield into Row freezing broken wall, obtains the lucidum spore powder of a broken wall;
S2, under the conditions of the lucidum spore powder of a broken wall is placed in -18 DEG C, after freezing embrittlement 3~5h, in 30~40 DEG C of conditions Under, supersonic wave wall breaking processing is carried out, the lucidum spore powder of secondary broken wall is obtained;
S3, the lucidum spore powder of the secondary broken wall of gained is placed in flash extracter, according to 1g:The past spirit of the ratio of 10~30mL After 2~3h of alcohol solution dipping that volumetric concentration is 75~85% is added in Ganoderma lucidum spore powder, 30~60S is handled at 30~50 DEG C Afterwards, it filters, obtains filtrate and filter residue;
Then according to 1g:The ethanol solution that volumetric concentration is 75~85% is added into filter residue for the ratio of 10~20mL, in 60 DEG C Lower ultrasonic 1~2h, filtering, merging filtrate, concentration and recovery ethyl alcohol obtain extracting solution;
S4, the extracting solution of gained is pumped into extraction tower, it is 1 then to press extracting solution with n-butanol volume ratio:1~3 ratio is past N-butanol is uniformly introduced in extraction tower carries out cycle high-speed counter-current extraction, control extraction temperature is 40~60 DEG C, cycling extraction 3~ After 5 times, extract liquor, concentration and recovery n-butanol are obtained, vacuum freeze drying obtains ganoderma spore polysaccharide.
2. a kind of ganoderma spore polysaccharide extraction process as described in claim 1, it is characterised in that:By ganoderma lucidum in the step S1 Spore is cut into the thin slice that thickness is 0.5mm.
3. a kind of ganoderma spore polysaccharide extraction process as described in claim 1, it is characterised in that:Ultrasound is broken in the step S2 The condition of wall is:Supersonic frequency is 18~24 kHz, and the time is 4~16mi n, and rotating speed is 20~50rpm.
4. a kind of ganoderma spore polysaccharide extraction process as described in claim 1, it is characterised in that:Supersonic frequency in the step S3 Rate is 120~180Hz.
CN201810839542.6A 2018-07-27 2018-07-27 A kind of ganoderma spore polysaccharide extraction process Pending CN108610435A (en)

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Cited By (5)

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CN110269172A (en) * 2019-07-29 2019-09-24 河北康平健康产业有限责任公司 Multidimensional health active peptide protein solid beverage
CN110698569A (en) * 2019-11-22 2020-01-17 福建拓天生物科技有限公司 Extraction process of polysaccharide in hericium erinaceus spore powder
CN111116773A (en) * 2020-03-02 2020-05-08 浙江养芝康生物科技有限公司 Ganoderma lucidum β glucan GLBG component and preparation process and application thereof
WO2020093510A1 (en) * 2018-11-06 2020-05-14 中科健康产业集团江苏药业有限公司 Separation and purification method for polysaccharide in ganoderma lucidum spores
CN111772044A (en) * 2020-08-03 2020-10-16 静宁县畜牧兽医中心 Beef cattle raising method for improving meat quality

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Publication number Priority date Publication date Assignee Title
WO2020093510A1 (en) * 2018-11-06 2020-05-14 中科健康产业集团江苏药业有限公司 Separation and purification method for polysaccharide in ganoderma lucidum spores
CN110269172A (en) * 2019-07-29 2019-09-24 河北康平健康产业有限责任公司 Multidimensional health active peptide protein solid beverage
CN110698569A (en) * 2019-11-22 2020-01-17 福建拓天生物科技有限公司 Extraction process of polysaccharide in hericium erinaceus spore powder
CN110698569B (en) * 2019-11-22 2021-05-25 福建拓天生物科技有限公司 Extraction process of polysaccharide in hericium erinaceus spore powder
CN111116773A (en) * 2020-03-02 2020-05-08 浙江养芝康生物科技有限公司 Ganoderma lucidum β glucan GLBG component and preparation process and application thereof
CN111772044A (en) * 2020-08-03 2020-10-16 静宁县畜牧兽医中心 Beef cattle raising method for improving meat quality

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Application publication date: 20181002