CN115261122A - Method for subcritical fluid extraction of ganoderma lucidum spore compound oil - Google Patents
Method for subcritical fluid extraction of ganoderma lucidum spore compound oil Download PDFInfo
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- CN115261122A CN115261122A CN202211067635.4A CN202211067635A CN115261122A CN 115261122 A CN115261122 A CN 115261122A CN 202211067635 A CN202211067635 A CN 202211067635A CN 115261122 A CN115261122 A CN 115261122A
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- ganoderma lucidum
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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
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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
- C11B1/04—Pretreatment of vegetable raw material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention provides a method for subcritical fluid extraction of ganoderma lucidum spore compound oil, which at least comprises the following steps: (1) pulverizing Ganoderma spore powder, semen Juglandis, ginseng radix seed, fructus Lycii and semen Hippophae at a certain ratio, and granulating; putting the ganoderma lucidum spore compound particles into an extraction tank, vacuumizing the extraction tank, and enabling the vacuum degree to be-0.1 MPa; introducing the subcritical fluid into an extraction tank, setting the extraction temperature to be 30-50 ℃ and the extraction time to be 2-12 hours; after extraction, introducing the subcritical fluid in the extraction tank into a separation tank for separation so as to extract effective components in the compound particles; collecting the ganoderma lucidum spore compound oil from the bottom of the separation tank, and recovering the subcritical fluid in the separation tank for recycling. The wall-broken ganoderma lucidum spore powder compound particles are extracted by subcritical fluid to obtain ganoderma lucidum spore compound oil, the product quality is good, the production process is environment-friendly and pollution-free, compared with the existing supercritical carbon dioxide fluid extraction, the equipment pressure is low, the production cost is low, and the method is extremely suitable for large-scale industrial operation.
Description
Technical Field
The invention relates to the technical field of ganoderma spore oil extraction, in particular to a method for subcritical fluid extraction of ganoderma spore compound oil.
Background
Ganoderma lucidum is a traditional rare medicinal material for strengthening body resistance, consolidating constitution, nourishing and strengthening. The ganoderma lucidum spores are germ cells which are continuously sprayed from the pileus of the ganoderma lucidum in the maturation period, and are seeds for breeding the next generation of the ganoderma lucidum, and in recent years, ganoderma lucidum spore oil has been developed into various high-grade health care products, and has very important medical value and economic value. The most commonly used extraction methods of ganoderma lucidum spore oil include organic solvent extraction and supercritical CO2 extraction. The supercritical CO2 fluid has better solubility to the active ingredients of the ganoderma lucidum spores, the CO2 has the characteristics of no color, no odor, no toxicity, no flammability and no explosion, and the problem of solvent residue after extraction is solved, so the supercritical CO2 fluid extraction process is widely applied to large-scale production. However, the supercritical CO2 extraction process needs to be completed under relatively extreme conditions, such as the process pressure needs to reach 30MPa-35MPa, and the extraction time is relatively long, so that industrialization is difficult to realize. The process can damage the active components of Ganoderma spore to a certain extent in the whole preparation process, and has high extraction cost. From the development trend of the ganoderma lucidum spore oil-related health-care food, the demand for the ganoderma lucidum spore oil and the compound oil is gradually expanded in the future, and a method capable of quickly and efficiently extracting the ganoderma lucidum spore oil and the compound oil is developed, so that the method has obvious practical significance and application value.
Disclosure of Invention
In view of the above-mentioned defects in the prior art, the technical problem to be solved by the present invention is to provide a method for subcritical fluid extraction of ganoderma lucidum spore compound oil, so as to solve the problems in the background art.
In order to solve the problems, the invention provides a method for subcritical fluid extraction of ganoderma lucidum spore compound oil, which at least comprises the following processes:
(1) compound granulation: taking one granule as a unit for measurement, selecting compound oil raw materials of 50-60% of ganoderma lucidum spore powder, 20-30% of walnut kernel, and 10-30% of ginseng seed, medlar and sea buckthorn seed which are uniformly proportioned in total measurement, crushing the raw materials, mixing and granulating to form ganoderma lucidum spore compound granules, wherein the diameter of the prepared granules is 1-3mm;
(2) placing the ganoderma lucidum spore compound particles formed in the step (1) into an extraction tank, and vacuumizing the extraction tank until the vacuum degree is-0.1 MPa; introducing the subcritical fluid into an extraction tank, setting the extraction temperature to be 30-50 ℃ and the extraction time to be 2-12 hours;
(3) after extraction, subcritical fluid in the extraction tank is introduced into a separation tank without decompression for separation so as to extract effective components in the compound particles;
(4) collecting the ganoderma lucidum spore compound oil from the bottom of the separation tank, and recovering the subcritical fluid in the separation tank for recycling.
Further, in the compound granulation of the step (1), the ganoderma lucidum spore powder and the walnut kernel particles are used as main raw materials, the ginseng seeds, the medlar and the seabuckthorn seeds are used as auxiliary raw materials, and the mixture is prepared according to a certain proportion by monarch, minister, assistant and guide.
Further, in the compound granulation of the above (1), the raw material mixture ratio of the unit ganoderma lucidum spore compound granule is preferably 50% of ganoderma lucidum spore powder, 20% of walnut kernel, 10% of ginseng seed, 10% of medlar and 10% of sea buckthorn seed.
Further, in the compound granulation of (1), the wall-broken ganoderma lucidum spore powder is selected as the ganoderma lucidum spore powder.
Further, in the compound granulation of the above (1), granulation with an equal size is performed by a granulator.
Further, the subcritical fluid medium introduced in (2) above may include one or a mixture of plural kinds of butane, tetrafluoroethane, propane, ethane and methane.
The invention also provides ganoderma spore compound oil which is prepared by the method for extracting the ganoderma spore compound oil through subcritical fluid.
The invention also provides a ganoderma lucidum spore compound oil product which comprises the ganoderma lucidum spore compound oil prepared by the method for extracting the ganoderma lucidum spore compound oil by subcritical fluid.
By implementing the method for extracting the ganoderma lucidum spore compound oil by subcritical fluid, provided by the invention, the following technical effects are achieved: the wall-broken ganoderma lucidum spore powder compound particles are extracted by subcritical fluid to obtain ganoderma lucidum spore compound oil, the product quality is good, the production process is environment-friendly and pollution-free, compared with the existing supercritical carbon dioxide fluid extraction, the equipment pressure is low, the production cost is low, and the method is extremely suitable for large-scale industrial operation.
Drawings
The conception, the specific structure and the technical effects of the present invention will be further described with reference to the accompanying drawings to fully understand the objects, the features and the effects of the present invention.
FIG. 1 is a process flow chart of the method for subcritical fluid extraction of ganoderma lucidum spore compound oil.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The technical solution of the present invention is described in detail below using examples.
The method for extracting the ganoderma lucidum spore compound oil by subcritical fluid as shown in figure 1 is characterized in that raw materials are firstly screened for preparing the compound oil, the ganoderma lucidum spores are seeds of the ganoderma lucidum which are extremely tiny oval germ cells ejected from ganoderma lucidum folds in the growth and maturation period of the ganoderma lucidum, and the ganoderma lucidum spore has extremely high medicinal and health-care values in the aspects of protecting cardiovascular vessels, reducing blood sugar, improving neurasthenia and the like, and is one of the main raw materials for preparing the compound oil; the traditional ganoderma lucidum spore oil contains unstable unsaturated fatty acid and is easy to deform, and the walnut kernel contains protein and walnut polyphenol, so that the walnut kernel has good antioxidant activity, the activity of removing free radicals can be enhanced, and the oxidative damage of the unsaturated fatty acid can be reduced, therefore, the ganoderma lucidum spore oil is matched with ganoderma lucidum spore powder in a certain proportion, and the health-care effect of the ganoderma lucidum spore compound oil can be more effectively improved; meanwhile, ginseng seeds, medlar and sea buckthorn seeds are obtained, and the compound oil is prepared by effectively utilizing the function of enhancing the immunity of the ginseng seeds and the medlar and the effect of the vitamins rich in the sea buckthorn seeds in assisting the cooperation with ganoderma lucidum spore powder according to a certain proportion.
Based on the selection of the raw materials of the ganoderma lucidum spore compound oil, the process for preparing the compound oil at least comprises the following working procedures:
(1) compound granulation: taking a granule as a unit for measurement, selecting 50-60% of ganoderma lucidum spore powder and 20-30% of walnut kernel as compound oil raw materials, and 10-30% of ginseng seed, medlar and seabuckthorn seed which are uniformly proportioned in total amount, crushing the raw materials, mixing and granulating to form ganoderma lucidum spore compound granules, wherein the prepared granules have the diameter of 1-3mm;
(2) placing the ganoderma lucidum spore compound particles formed in the step (1) into an extraction tank, and vacuumizing the extraction tank until the vacuum degree is-0.1 MPa; introducing the subcritical fluid into an extraction tank, setting the extraction temperature to be 30-50 ℃ and the extraction time to be 2-12 hours;
(3) after extraction, subcritical fluid in the extraction tank is introduced into a separation tank without decompression for separation so as to extract effective components in the compound particles;
(4) collecting the ganoderma lucidum spore compound oil from the bottom of the separation tank, and recovering the subcritical fluid in the separation tank for recycling.
This solution is further illustrated in the following examples:
example 1
Firstly, because the ganoderma lucidum spore has an outer wall which is formed by a layer of chitin which is extremely difficult to be digested by gastric acid of a human body, the ganoderma lucidum spore needs to be subjected to wall breaking treatment, the outer wall of the layer is opened, the effective components tightly wrapped by the outer wall can be utilized and absorbed by the human body to the maximum extent, and meanwhile, walnut kernels, ginseng seeds, medlar and sea buckthorn seeds are obtained;
secondly, blending the obtained wall-broken ganoderma lucidum spore powder, walnut kernels, ginseng seeds, wolfberry fruits and sea buckthorn seeds according to the ratio of 5;
thirdly, placing the granules manufactured by the granulator in an extraction tank, vacuumizing the extraction tank, introducing subcritical fluid butane into the extraction tank from a liquid storage tank after the vacuum degree is reduced to-0.1 MPa, setting the extraction temperature to be 50 ℃, and setting the extraction time to be 2 hours;
fourthly, after extraction is finished, introducing subcritical fluid butane in the extraction tank into a separation tank for separation so as to extract effective components in the compound particles;
and finally, collecting the separated ganoderma lucidum spore compound oil from the bottom of the separation tank, and recycling subcritical fluid butane in the separation tank through a condensation tank.
The basic structures of the granulator, the separating tank, the extraction tank, the liquid storage tank and the condensing tank used in the above steps can be the same as those of the existing granulator, separating tank, extraction tank, liquid storage tank and condensing tank, and are not described in detail herein.
Example 2
Firstly, because the ganoderma lucidum spore has an outer wall formed by chitin which is extremely difficult to be digested by gastric acid of a human body, the ganoderma lucidum spore needs to be subjected to wall breaking treatment, the outer wall of the layer is opened, the effective components tightly wrapped by the outer wall can be furthest utilized and absorbed by the human body, and meanwhile, walnut kernels, ginseng seeds, wolfberry fruits and sea buckthorn seeds are obtained;
secondly, blending the obtained wall-broken ganoderma lucidum spore powder, walnut kernels, ginseng seeds, wolfberry fruits and sea buckthorn seeds according to the proportion of 6;
thirdly, placing the granules manufactured by the granulator in an extraction tank, vacuumizing the extraction tank, introducing subcritical fluid butane into the extraction tank from a liquid storage tank after the vacuum degree is reduced to-0.1 MPa, setting the extraction temperature to be 40 ℃, and setting the extraction time to be 2 hours;
fourthly, after extraction is finished, introducing subcritical fluid tetrafluoroethane in the extraction tank into a separation tank for separation so as to extract effective ingredients in the compound particles;
and finally, collecting the separated ganoderma spore compound oil from the bottom of the separation tank, and recovering subcritical fluid tetrafluoroethane in the separation tank through a condensation tank for recycling.
Example 3
Firstly, because the ganoderma lucidum spore has an outer wall formed by chitin which is extremely difficult to be digested by gastric acid of a human body, the ganoderma lucidum spore needs to be subjected to wall breaking treatment, the outer wall of the layer is opened, the effective components tightly wrapped by the outer wall can be furthest utilized and absorbed by the human body, and meanwhile, walnut kernels, ginseng seeds, wolfberry fruits and sea buckthorn seeds are obtained;
secondly, blending the obtained wall-broken ganoderma lucidum spore powder, walnut kernels, ginseng seeds, medlar and sea buckthorn seeds according to the proportion of 5/3;
thirdly, placing the granules manufactured by the granulator in an extraction tank, vacuumizing the extraction tank, introducing subcritical fluid butane into the extraction tank from a liquid storage tank after the vacuum degree is reduced to-0.1 MPa, setting the extraction temperature to be 30 ℃, and setting the extraction time to be 2 hours;
fourthly, after extraction is finished, introducing subcritical fluid propane in the extraction tank into a separation tank for separation so as to extract effective components in the compound particles;
and finally, collecting the separated ganoderma lucidum spore compound oil from the bottom of the separation tank, and recycling subcritical fluid propane in the separation tank through a condensation tank.
Example 4
Firstly, because the ganoderma lucidum spore has an outer wall formed by chitin which is extremely difficult to be digested by gastric acid of a human body, the ganoderma lucidum spore needs to be subjected to wall breaking treatment, the outer wall of the layer is opened, the effective components tightly wrapped by the outer wall can be furthest utilized and absorbed by the human body, and meanwhile, walnut kernels, ginseng seeds, wolfberry fruits and sea buckthorn seeds are obtained;
secondly, blending the obtained wall-broken ganoderma lucidum spore powder, walnut kernels, ginseng seeds, medlar and sea buckthorn seeds according to the ratio of 2/3;
thirdly, placing the granules manufactured by the granulator in an extraction tank, vacuumizing the extraction tank, introducing subcritical fluid butane into the extraction tank from a liquid storage tank after the vacuum degree is reduced to-0.1 MPa, setting the extraction temperature to be 30 ℃, and setting the extraction time to be 2 hours;
fourthly, after extraction is finished, introducing subcritical fluid methane in the extraction tank into a separation tank for separation so as to extract effective components in the compound particles;
and finally, collecting the separated ganoderma lucidum spore compound oil from the bottom of the separation tank, and recycling subcritical fluid tetrafluoroethane in the separation tank through a condensation tank for recycling.
Example 5
Firstly, because the ganoderma lucidum spore has an outer wall which is formed by a layer of chitin which is extremely difficult to be digested by gastric acid of a human body, the ganoderma lucidum spore needs to be subjected to wall breaking treatment, the outer wall of the layer is opened, the effective components tightly wrapped by the outer wall can be utilized and absorbed by the human body to the maximum extent, and meanwhile, walnut kernels, ginseng seeds, medlar and sea buckthorn seeds are obtained;
secondly, blending the obtained wall-broken ganoderma lucidum spore powder, walnut kernels, ginseng seeds, wolfberry fruits and sea buckthorn seeds according to the proportion of 5;
thirdly, placing the granules manufactured by the granulator in an extraction tank, vacuumizing the extraction tank, introducing subcritical fluid butane into the extraction tank from a liquid storage tank after the vacuum degree is reduced to-0.1 MPa, setting the extraction temperature to be 50 ℃, and setting the extraction time to be 2 hours;
fourthly, after extraction is finished, introducing subcritical fluid ethane in the extraction tank into a separation tank for separation so as to extract effective components in the compound particles;
and finally, collecting the separated ganoderma lucidum spore compound oil from the bottom of the separation tank, and recycling subcritical fluid ethane in the separation tank through a condensation tank for recycling.
It should be added that, unless otherwise defined, technical or scientific terms used herein shall have the ordinary meaning as understood by those of ordinary skill in the art to which this invention belongs. .
Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. This application is intended to cover any uses or adaptations of the invention following, in general, the principles of the invention and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the invention being indicated by the following claims.
It will be understood that the present invention is not limited to the structures that have been described above and shown in the drawings, and that various modifications and changes can be made without departing from the scope thereof. The scope of the invention is limited only by the appended claims.
Claims (8)
1. A method for subcritical fluid extraction of ganoderma lucidum spore compound oil is characterized by at least comprising the following processes:
(1) compound granulation: taking a granule as a unit for measurement, selecting 50-60% of ganoderma lucidum spore powder and 20-30% of walnut kernel as compound oil raw materials, and 10-30% of ginseng seed, medlar and seabuckthorn seed which are uniformly proportioned in total amount, crushing the raw materials, mixing and granulating to form ganoderma lucidum spore compound granules, wherein the prepared granules have the diameter of 1-3mm;
(2) placing the ganoderma lucidum spore compound particles formed in the step (1) into an extraction tank, and vacuumizing the extraction tank until the vacuum degree is-0.1 MPa; introducing the subcritical fluid into an extraction tank, setting the extraction temperature to be 30-50 ℃ and the extraction time to be 2-12 hours;
(3) after extraction, subcritical fluid in the extraction tank is introduced into a separation tank without decompression for separation so as to extract effective components in the compound particles;
(4) collecting the ganoderma lucidum spore compound oil from the bottom of the separation tank, and recovering the subcritical fluid in the separation tank for recycling.
2. The subcritical fluid extraction method of ganoderma lucidum spore compound oil according to claim 1, wherein in the compound granulation of (1), ganoderma lucidum spore powder and walnut kernel particles are used as main raw materials, and ginseng seeds, medlar and sea buckthorn seeds are used as auxiliary raw materials, and are matched in a certain proportion according to monarch, minister, assistant and guide compatibility.
3. The method for subcritical fluid extraction of ganoderma lucidum spore compound oil according to claim 2, wherein in the compound granulation of (1), the raw material mixture ratio of the unit ganoderma lucidum spore compound granule is preferably 50% of ganoderma lucidum spore powder, 20% of walnut kernel, 10% of ginseng seed, 10% of wolfberry fruit and 10% of sea buckthorn seed.
4. The subcritical fluid extraction method of ganoderma lucidum spore compound oil according to claim 3, wherein in the compound granulation of (1), ganoderma lucidum spore powder is wall-broken ganoderma lucidum spore powder.
5. The method for subcritical fluid extraction of ganoderma lucidum spore compound oil according to claim 4, wherein granulation with equal size is performed in the compound granulation of (1) above by a granulator.
6. The method for subcritical fluid extraction of ganoderma lucidum spore compound oil according to claim 5, wherein the subcritical fluid medium introduced in (2) comprises one or more of butane, tetrafluoroethane, propane, ethane and methane.
7. A ganoderma spore compound oil, characterized in that the ganoderma spore compound oil is prepared by the subcritical fluid extraction method of ganoderma spore compound oil according to any one of claims 1 to 6.
8. A ganoderma spore compound oil product is characterized in that the ganoderma spore compound oil product comprises the ganoderma spore compound oil of claim 7, and the ganoderma spore compound oil is prepared by the method for extracting the ganoderma spore compound oil from the subcritical fluid of any one of claims 1 to 6.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104531341A (en) * | 2014-12-18 | 2015-04-22 | 贵州航天乌江机电设备有限责任公司 | Process for extracting ganoderma lucidum spore oil through supercritical method |
| CN104845732A (en) * | 2015-05-06 | 2015-08-19 | 福建荣安天然植物开发有限公司 | Method for efficiently extracting ganoderma lucidum spores oil by using subcritical mixed solvent |
| CN106962506A (en) * | 2017-04-13 | 2017-07-21 | 张鸣 | A kind of ready-mixed oil and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104531341A (en) * | 2014-12-18 | 2015-04-22 | 贵州航天乌江机电设备有限责任公司 | Process for extracting ganoderma lucidum spore oil through supercritical method |
| CN104845732A (en) * | 2015-05-06 | 2015-08-19 | 福建荣安天然植物开发有限公司 | Method for efficiently extracting ganoderma lucidum spores oil by using subcritical mixed solvent |
| CN106962506A (en) * | 2017-04-13 | 2017-07-21 | 张鸣 | A kind of ready-mixed oil and preparation method thereof |
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