CN106867657A - A kind of efficient, multi-stage supercritical CO2The method of Ganoderma Lucidum Spores Oil Extracted - Google Patents
A kind of efficient, multi-stage supercritical CO2The method of Ganoderma Lucidum Spores Oil Extracted Download PDFInfo
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- CN106867657A CN106867657A CN201710161927.7A CN201710161927A CN106867657A CN 106867657 A CN106867657 A CN 106867657A CN 201710161927 A CN201710161927 A CN 201710161927A CN 106867657 A CN106867657 A CN 106867657A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/025—Pretreatment by enzymes or microorganisms, living or dead
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Abstract
The present invention relates to traditional Chinese medicine ingredients extractive technique field, specifically related to a kind of method that ganoderma lucidum spore oil is prepared through ultramicro grinding and biological enzyme combined wall breakage, microwave reinforced SCF-CO 2 as raw material with Reishi sporule, the ultramicro grinding that the present invention is used and biological enzyme combined wall breakage technology, not only improve sporoderm-broken rate, and improve broken wall efficiency, more single broken wall method broken wall efficiency improves 30%~50%, and sporoderm-broken rate is up to more than 99.7%；The microwave reinforced SCF-CO 2 for using, can complete extraction, easy to operate, low cost under relatively mild environment；The Reishi sporule is through ultramicro grinding and biological enzyme combined wall breakage, wet granulation, microwave reinforced SCF-CO 2, gained ganoderma lucidum spore oil oil yield is 41.3%, high compared with SCF-CO 2 oil yield by 17.1%, the bioactive ingredients such as ganodenic acid, ergosterol content can improve 10%~20%.
Description
Technical field
The present invention relates to traditional Chinese medicine ingredients extractive technique field, and in particular to it is a kind of with Reishi sporule be raw material through ultramicro grinding
The method for preparing ganoderma lucidum spore oil with biological enzyme combined wall breakage, microwave reinforced SCF-CO 2.
Background technology
Ganoderma lucidum has very long history as medicine, early in the Eastern Han Dynasty, first medicine works of China《The legendary god of farming
Book on Chinese herbal medicine warp》Described in：Ganoderma lucidum has purple, red, blue or green, yellow, white, black six kinds, and property sweet taste cures mainly and " ties in the heart, the beneficial motive, bowl spares, increase
Wisdom, does not forget, and food is made light of one's life by commiting suicide not always long, macrobiosis angle ", and ganoderma lucidum is classified as top grade.《Pharmacopoeia of People's Republic of China》Year version one
Portion records the function of Ganoderma lucidum and cures mainly：Invigorating qi for tranquilization, it is relieving cough and asthma.For having no peace of mind, palpitaition of having a sleepless night, deficiency syndrome of the lung cough and asthma,
Consumptive disease is losed heart, do not feel like eating.Successively approval ganoderma lucidum is health food for health ministry, State Food and Drug Administration, its
Major function has：Strengthen body immunity, anti-aging, improve the health care of sleep, suppress tumour.
Reishi sporule is that the reproduction cell load of ganoderma lucidum is embraced a son and is commonly called as ganoderma lucidum seed, is ganoderma lucidum in growth and maturity period from cap
And the extremely tiny particle for ejecting, Reishi sporule is presented powdered after putting together, is commonly referred to as lucidum spore powder.Spirit
Ganoderma lucidum spore contains the whole genetic activities material of ganoderma lucidum.The active ingredient of Reishi sporule is very enriched, and contains polysaccharide, triterpene
Various bioactive ingredients such as class, protein and amino acids, vitamins, alkaloids and fatty acid, wherein spirit
Sesame polysaccharide and triterpene compound are more counted as its main active material, with various biological functions, such as resist
Tumour and anti-good fortune penetrate function, anti-cardiovascular disease, nervous system regulatory function, resisting oxygen lack, it is anti-oxidant, removing toxic substances liver protection and
Immune-enhancing effect etc. is acted on.
It is strong but pliable in texture, acidproof with layered network because the sporoderm of Reishi sporule is made up of chitin and glucan
Alkali, it is extremely difficult to oxidation Decomposition, if do not decomposed, its internal active component is difficult to be extracted, also be difficult to after human body is edible by
Digest and assimilate.Therefore in order to make full use of the active component in Reishi sporule, it is necessary to carry out broken wall to Reishi sporule wall, then adopt
Extracted with the modern times and isolation technics, the active component in enrichment Reishi sporule gives full play to ganoderma lucidum medicinal efficacy.
Current ganoderma lucidium spore powder wall breaking technology is mainly Mechanical Method and biological enzyme, and biological enzyme is compared with Mechanical Method broken wall efficiency
Using lucidum strain is accessed in height, such as Chinese patent CN100593410C, using the fiber that it constantly secretes in growth course
The complex enzyme zymohydrolysis conidial cell wall such as plain enzyme, pectase, this method is relatively mild, but the more difficult control of process, and required time is more long.Ganoderma lucidum
Spore oil extractive technique reports that more is CO_2 supercritical technology, such as CN144536A, CN1094766C, with tradition side
Method is compared, and has with short production cycle, active ingredient survivable, no solvent residue, it is free from environmental pollution the advantages of.Even so, super
Critical CO2 abstraction techniques Ganoderma Lucidum Spores Oil Extracted needs pressure and extraction time more long higher, due to lucidum spore powder powder
Body is thinner, and material spray is easily caused under elevated pressure conditions, not only influences the extraction quality of spore oil, and hidden with production safety
Suffer from.To solve this problem, in the prior art using method of granulating, with spore powder with crushed sporoderm as former in such as patent CN1239100C
Material, through the granulation of the ethanol water of volume ratio 5%~95%, dries, and because ethanol is inflammable, has in drying process and is absolutely unsafe
Factor.With conidia powder as raw material in patent CN1094766C, through the method for water, gelatin, starch extrusion forming at room temperature, this method
More auxiliary material is added, spore oil extraction efficiency is not only influenceed, and more pollutions may be brought.
The content of the invention
The present invention is directed to problems of the prior art, there is provided a kind of efficient, multi-stage supercritical CO2 extracting ganoderma spores
The method of oil, using ultramicro grinding and biological enzyme combined wall breakage in this method, through wet granulation, by microwave reinforced overcritical
CO2 is obtained by extraction ganoderma lucidum spore oil, and with reaching, broken time is short, sporoderm-broken rate is high, and pressure is small, temperature is low needed for extraction, extraction
Time is short, oil yield advantage high.
The present invention is achieved through the following technical solutions the purpose：
A kind of efficient, method of multi-stage supercritical CO2 Ganoderma Lucidum Spores Oil Extracteds, comprises the following steps：
Step A, selection Reishi sporule, dry 5 hours at 40 DEG C；
Step B, the Reishi sporule that step A is obtained is put into micronizer and is crushed, obtain just wall-breaking lucidum spore
Sub- powder；
Step C, the conidia powder for obtaining step B mixes with biology enzyme carries out enzymolysis broken wall, and biological enzyme dosage is 0.1%~
0.5%, hydrolysis temperature is 25~45 DEG C, pH value 4.5~8.5, and enzymolysis time is 0.5~3 hour；
Step D, wet granulation is carried out to adding wetting agent in step C miospore powder, it is 20 that grain diameter is obtained after drying
~60 mesh, particle of the moisture less than 5%；
Step E, step D miospore powder particles are put into the SCF-CO 2 kettle equipped with microwave generator, make its with
Supercritical fluid is fully contacted, dissolves, extracts, separates, wherein extracting pressure be 15~35MPa, extraction temperature be 30~50 DEG C,
CO2 fluid flows are 15~60L/h, extraction time 30~150 minutes；
Step F, by the spore oil in step E by 12000 revs/min of high speed centrifugations be obtained refining ganoderam lucidum spore oil.
Used as preferred, grinding time is 10~40 minutes in micronizer in the step B.
Used as preferred, the biology enzyme in the step C is cellulase, pectase, hemicellulase, lywallzyme, egg
Any one or more complex enzyme in white matter enzyme.
Used as preferred, the wetting agent in the step D is purified water, and drying temperature is 35 DEG C.
Wherein, in the step E, one-level separating pressure is 7~9MPa, separation temperature is 30~50 DEG C, the second-order separation pressure
Power is 4~7MPa, separation temperature is 30~50 DEG C.
Further, the extraction process of the step E adds entrainer, and the entrainer is that absolute ethyl alcohol or ethanol are water-soluble
Liquid.
Compared with prior art, the present invention has the advantages that：
1. the present invention is used ultramicro grinding and biological enzyme combined wall breakage technology, not only improve sporoderm-broken rate, and improve
Broken wall efficiency, more single broken wall method broken wall efficiency improves 30%~50%, and sporoderm-broken rate is up to more than 99.7%；
2. the microwave reinforced SCF-CO 2 that the present invention is used, preferably extracting pressure are 25MPa, and extraction temperature is 35
DEG C, CO2 flows are 25L/h, and extraction time is 120 minutes, low compared with condition needed for SCF-CO 2, in relatively mild ring
Extraction, easy to operate, low cost can be completed under border；
3. in the present invention Reishi sporule through ultramicro grinding and biological enzyme combined wall breakage, wet granulation, microwave reinforced super face
Boundary CO2 is extracted, and gained ganoderma lucidum spore oil oil yield is 41.3%, high compared with SCF-CO 2 oil yield by 17.1%, ganoderma lucidum three
The bioactive ingredients such as terpene, ergosterol content can improve 10%~20%.
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail.
Embodiment 1.
A kind of method that efficient, multi-stage supercritical CO2 extractions prepare ganoderma lucidum spore oil, its preparation method is as follows：
Step A, preferably Reishi sporule, dry 5 hours at 4 DEG C；
Step B, the Reishi sporule that step A is obtained is put into micronizer and is crushed 40 minutes, obtains just wall-breaking lucidum
Conidia powder；
Step C, the conidia powder that step B is obtained digests broken wall with biology enzyme in suitable condition, and wherein biology enzyme is fiber
Any one or more complex enzyme in plain enzyme, pectase, hemicellulase, lywallzyme, protease etc., biological enzyme dosage is
0.2%, suitable condition is temperature 45 C, and pH value 6.5, enzymolysis time is 3 hours；
Step D, wet granulation is carried out by step C miospores powder, is dried at 35 DEG C, obtains particle of the moisture less than 5%,
Wherein with purified water as wetting agent, grain diameter is 20~60 mesh；
Step E, step D miospore powder particles are put into the SCF-CO 2 kettle equipped with microwave generator, make its with
Supercritical fluid is fully contacted, dissolves, extracts, separates, wherein extracting pressure be 15MPa, extraction temperature be 50 DEG C, CO2 fluids
Flow is 15L/h, extraction time 150 minutes.One-level separating pressure is 7.5MPa, separation temperature is 50 DEG C, the second-order separation pressure
For 4MPa, separation temperature are 50 DEG C, extraction process can also add entrainer, such as absolute ethyl alcohol；
Step F, refining ganoderam lucidum spore oil is obtained by the spore oil in step E by 12000 revs/min of high speed centrifugations.
Embodiment 2.
A kind of method that efficient, multi-stage supercritical CO2 extractions prepare ganoderma lucidum spore oil, its preparation method is as follows：
Step A, preferably Reishi sporule, dry 5 hours at 4 DEG C；
Step B, the Reishi sporule that step A is obtained is put into micronizer and is crushed 30 minutes, obtains just wall-breaking lucidum
Conidia powder；
Step C, the conidia powder that step B is obtained digests broken wall with biology enzyme in suitable condition, and wherein biology enzyme is fiber
Any one or more complex enzyme in plain enzyme, pectase, hemicellulase, lywallzyme, protease etc., biological enzyme dosage is
0.1%, suitable condition is 25 DEG C of temperature, and pH value 4.5, enzymolysis time is 1 hour；
Step D, wet granulation is carried out by step C miospores powder, is dried at 35 DEG C, obtains particle of the moisture less than 5%,
Wherein with purified water as wetting agent, grain diameter is 20~60 mesh；
Step E, step D miospore powder particles are put into the SCF-CO 2 kettle equipped with microwave generator, make its with
Supercritical fluid is fully contacted, dissolves, extracts, separates, wherein extracting pressure be 20MPa, extraction temperature be 45 DEG C, CO2 fluids
Flow is 20L/h, extraction time 75 minutes.One-level separating pressure is 8MPa, separation temperature is 45 DEG C, and the second-order separation pressure is
5MPa, separation temperature are 45 DEG C, and extraction process can also add entrainer, such as ethanol water；
Step F, refining ganoderam lucidum spore oil is obtained by the spore oil in step E by 12000 revs/min of high speed centrifugations.
Embodiment 3.
A kind of method that efficient, multi-stage supercritical CO2 extractions prepare ganoderma lucidum spore oil, its preparation method is as follows：
Step A, preferably Reishi sporule, dry 5 hours at 40 DEG C；
Step B, the Reishi sporule that step A is obtained is put into micronizer and is crushed 20 minutes, obtains just wall-breaking lucidum
Conidia powder；
Step C, the conidia powder that step B is obtained digests broken wall with biology enzyme in suitable condition, and wherein biology enzyme is fiber
One or more complex enzyme in plain enzyme, pectase, hemicellulase, lywallzyme, protease etc., biological enzyme dosage is
0.3%, suitable condition is 38 DEG C of temperature, and pH value 5.5, enzymolysis time is 2 hours；
Step D, wet granulation is carried out by step C miospores powder, is dried at 35 DEG C, obtains particle of the moisture less than 5%,
Wherein with purified water as wetting agent, grain diameter is 20~60 mesh；
Step E, step D miospore powder particles are put into the SCF-CO 2 kettle equipped with microwave generator, make its with
Supercritical fluid is fully contacted, dissolves, extracts, separates, wherein extracting pressure be 25MPa, extraction temperature be 35 DEG C, CO2 fluids
Flow is 25L/h, extraction time 120h.One-level separating pressure is 8.5MPa, separation temperature is 35 DEG C, and the second-order separation pressure is
6.5MPa, separation temperature are 35 DEG C, and extraction process can also add entrainer, such as absolute ethyl alcohol or ethanol water；
Step F, refining ganoderam lucidum spore oil is obtained by the spore oil in step E by 12000 revs/min of high speed centrifugations.
Embodiment 4.
A kind of method that efficient, multi-stage supercritical CO2 extractions prepare ganoderma lucidum spore oil, its preparation method is as follows：
Step A, preferably Reishi sporule, dry 5 hours at 40 DEG C；
Step B, the Reishi sporule that step A is obtained is put into micronizer and is crushed 10 minutes, obtains just wall-breaking lucidum
Conidia powder；
Step C, the conidia powder that step B is obtained digests broken wall with biology enzyme in suitable condition, and wherein biology enzyme is fiber
One or more complex enzyme in plain enzyme, pectase, hemicellulase, lywallzyme, protease etc., biological enzyme dosage is
0.5%, suitable condition is 30 DEG C of temperature, and pH value 8.5, enzymolysis time is 0.5 hour；
Step D, wet granulation is carried out by step C miospores powder, is dried at 35 DEG C, obtains particle of the moisture less than 5%,
Wherein with purified water as wetting agent, grain diameter is 20~60 mesh；
Step E, step D miospore powder particles are put into the SCF-CO 2 kettle equipped with microwave generator, make its with
Supercritical fluid is fully contacted, dissolves, extracts, separates, wherein extracting pressure be 35MPa, extraction temperature be 30 DEG C, CO2 fluids
Flow is 45L/h, extraction time 30 minutes.One-level separating pressure is 9MPa, separation temperature is 30 DEG C, and the second-order separation pressure is
7MPa, separation temperature are 30 DEG C, and extraction process can also add entrainer, such as absolute ethyl alcohol or ethanol water；
Step F, refining ganoderam lucidum spore oil is obtained by the spore oil in step E by 12000 revs/min of high speed centrifugations.
Embodiment described above only expresses several embodiments of the invention, and its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Shield scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (6)
1. it is a kind of efficiently, the method for multi-stage supercritical CO2 Ganoderma Lucidum Spores Oil Extracteds, it is characterised in that comprise the following steps：
Step A, selection Reishi sporule, dry 5 hours at 40 DEG C；
Step B, the Reishi sporule that step A is obtained is put into micronizer and is crushed, obtain just ganoderma spove powder；
Step C, the conidia powder for obtaining step B mixes with biology enzyme carries out enzymolysis broken wall, and biological enzyme dosage is 0.1%~
0.5%, hydrolysis temperature is 25~45 DEG C, pH value 4.5~8.5, and enzymolysis time is 0.5~3 hour；
Step D, wet granulation is carried out to adding wetting agent in step C miospore powder, it is 20~60 that grain diameter is obtained after drying
Mesh, particle of the moisture less than 5%；
Step E, step D miospore powder particles are put into the SCF-CO 2 kettle equipped with microwave generator, it is faced with super
Boundary's fluid is fully contacted, dissolves, extracts, separates, wherein extracting pressure be 15~35MPa, extraction temperature be 30~50 DEG C, CO2
Fluid flow is 15~60L/h, extraction time 30~150 minutes；
Step F, by the spore oil in step E by 12000 revs/min of high speed centrifugations be obtained refining ganoderam lucidum spore oil.
2. it is according to claim 1 efficiently, the method for multi-stage supercritical CO2 Ganoderma Lucidum Spores Oil Extracteds, it is characterised in that institute
State in step B that grinding time is 10~40 minutes in micronizer.
3. the quick preparation technology of Desert Herba Cistanches extract according to claim 1, it is characterised in that the step C
In biology enzyme be combined for any one or more in cellulase, pectase, hemicellulase, lywallzyme, protease
Enzyme.
4. the quick preparation technology of Desert Herba Cistanches extract according to claim 1, it is characterised in that the step D
In wetting agent be purified water, drying temperature be 35 DEG C.
5. the quick preparation technology of Desert Herba Cistanches extract according to claim 1, it is characterised in that the step E
In, one-level separating pressure is 7~9MPa, separation temperature is 30~50 DEG C, and the second-order separation pressure is 4~7MPa, separation temperature is
30~50 DEG C.
6. the quick preparation technology of Desert Herba Cistanches extract according to claim 1, it is characterised in that the step E
Extraction process add entrainer, the entrainer be absolute ethyl alcohol or ethanol water.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108192735A (en) * | 2018-01-17 | 2018-06-22 | 刘勇 | Plant extraction oil, the leach extraction method of plant extraction oil and application |
| CN109010399A (en) * | 2018-07-17 | 2018-12-18 | 广州今典精方医药科技有限公司 | A kind of preparation method of plant cell wall breaking powder |
| CN110558499A (en) * | 2019-09-19 | 2019-12-13 | 福建启元堂生物技术有限公司 | Pretreatment method for double-super-extraction of marine nutrients |
| CN110575680A (en) * | 2019-09-19 | 2019-12-17 | 福建启元堂生物技术有限公司 | Method for double super-extraction of marine nutrients |
| CN115282171A (en) * | 2022-08-13 | 2022-11-04 | 青海净草生物科技有限公司 | Ganoderma lucidum spore oil with immunity improving function and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108192735A (en) * | 2018-01-17 | 2018-06-22 | 刘勇 | Plant extraction oil, the leach extraction method of plant extraction oil and application |
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| CN110558499A (en) * | 2019-09-19 | 2019-12-13 | 福建启元堂生物技术有限公司 | Pretreatment method for double-super-extraction of marine nutrients |
| CN110575680A (en) * | 2019-09-19 | 2019-12-17 | 福建启元堂生物技术有限公司 | Method for double super-extraction of marine nutrients |
| CN115282171A (en) * | 2022-08-13 | 2022-11-04 | 青海净草生物科技有限公司 | Ganoderma lucidum spore oil with immunity improving function and preparation method thereof |
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Application publication date: 20170620 |