CN112587554B - Ganoderma lucidum spore oil with gastric mucosa protecting effect and preparation method and equipment thereof - Google Patents
Ganoderma lucidum spore oil with gastric mucosa protecting effect and preparation method and equipment thereof Download PDFInfo
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- CN112587554B CN112587554B CN202011478490.8A CN202011478490A CN112587554B CN 112587554 B CN112587554 B CN 112587554B CN 202011478490 A CN202011478490 A CN 202011478490A CN 112587554 B CN112587554 B CN 112587554B
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- GYYNKVUPNNEHDM-UHFFFAOYSA-N dibutyl benzene-1,2-dicarboxylate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC.CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC GYYNKVUPNNEHDM-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
- A61K36/06—Fungi, e.g. yeasts
- A61K36/07—Basidiomycota, e.g. Cryptococcus
- A61K36/074—Ganoderma
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
- A61P1/04—Drugs for disorders of the alimentary tract or the digestive system for ulcers, gastritis or reflux esophagitis, e.g. antacids, inhibitors of acid secretion, mucosal protectants
-
- 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
-
- 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
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
-
- 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
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mycology (AREA)
- Animal Behavior & Ethology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Veterinary Medicine (AREA)
- Medicinal Chemistry (AREA)
- Public Health (AREA)
- Pharmacology & Pharmacy (AREA)
- General Health & Medical Sciences (AREA)
- Alternative & Traditional Medicine (AREA)
- Epidemiology (AREA)
- Microbiology (AREA)
- Medical Informatics (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Botany (AREA)
- General Chemical & Material Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Biotechnology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
A ganoderma lucidum spore oil with protective effect on gastric mucosa is prepared by extracting ganoderma lucidum spore powder by supercritical carbon dioxide double extraction technology, wherein the acid value of ganoderma lucidum spore oil is less than or equal to 2KOH (mg/g), and the peroxide value is less than or equal to 0.1%. Extracting Ganoderma spore powder by supercritical carbon dioxide extraction to obtain Ganoderma spore crude oil, and purifying the Ganoderma spore crude oil by supercritical carbon dioxide extraction to obtain Ganoderma spore oil. The ganoderma lucidum spore oil has the function of protecting gastric mucosa, can obviously reduce gastric mucosa injury ulcer and hemorrhage caused by gastric mucosa injury agents such as ethanol, indomethacin and the like, and delays the occurrence time of ethanol effect. The glossy ganoderma spore oil has stable quality, and can be used as raw material of food, health food or medicine to protect gastric mucosa and prevent gastric mucosa from damaging ulcer and bleeding.
Description
Technical Field
The invention belongs to the field of natural product extraction and traditional Chinese medicine preparation, relates to the technical field of processing and utilization of ganoderma lucidum spores, and in particular relates to ganoderma lucidum spore oil with a protective effect on gastric mucosa and a preparation method thereof
Background
Ganoderma lucidum (Ganoderma lucidum (Leys. ExFr.) Karst.) is one of Ganoderma lucidum (part of Chinese pharmacopoeia 2015) belonging to Polyporaceae, and has sweet taste and is effective in strengthening body resistance and consolidating constitution. The Ganoderma spore powder is collection of Ganoderma spore of germ cells generated in mature period of Ganoderma fruiting body. Contains unsaturated fatty acids, sterols, triterpenes, alkaloids, lactones, proteins and amino acids, glycopeptides and inorganic salts.
The gastrointestinal tract is not only an important digestive organ of the human body, but also the largest immune system of the human body. The functions of digesting and absorbing nutrient substances and the like are exerted, and meanwhile, the external stimulus is prevented, and the organism is protected from being affected by harmful substances such as bacteria, toxins, medicines and the like. Clinically, various gastrointestinal diseases may damage the epithelium of the gastrointestinal mucosa, and further may develop into important gastrointestinal diseases such as inflammatory bowel disease. There is a very tight barrier between the gastric cavity and the gastric mucosal space, called the gastric mucosal barrier, which is made up of the tight junctions between the epithelial top cell membrane and adjacent cells. Under normal conditions, this barrier can prevent H in the gastric cavity + The gastric juice with extremely high acidity is prevented from damaging gastric mucosa by diffusing into the mucosa along the concentration difference to erode the mucosa layer. Certain substancesOr drugs such as aspirin, indomethacin, ethanol, acetic acid, cholic acid, etc., can destroy the gastric mucosal barrier. Once the barrier is damaged, H + It can quickly invade the mucous membrane to cause a series of pathological processes, leading to edema, hemorrhage and even necrosis of the mucous membrane and ulcer formation.
The supercritical carbon dioxide extraction technology is that supercritical carbon dioxide is contacted with substances to be separated under a supercritical state, so that components with polarity, boiling point, molecular weight and the like are selectively and sequentially extracted. The mixed components are obtained by controlling the conditions, then supercritical carbon dioxide is changed into gas by means of decompression and temperature rising and falling, and the extracted substances are automatically and completely separated out, so that the aim of separation and purification is achieved, and the extraction and separation processes are integrated.
The patent 'a pharmaceutical composition for treating gastrointestinal diseases and application thereof' (CN 110841027) is prepared from 10-30 parts of litsea cubeba oil, 20-40 parts of cloud sesame oil, 10-30 parts of linseed oil, 10-30 parts of sea buckthorn oil, 10-30 parts of fructus amomi, 5-15 parts of medlar seed oil and 5-15 parts of ganoderma lucidum spore oil according to a certain proportion, wherein the compound combination leads to undefined active ingredients which really exert the efficacy. At the same time, pharmacological results show that: compared with the normal group, the gastric mucosa is light red, and a little fur-like substance is arranged on the surface, which proves that the gastric mucosa is still damaged to a certain extent, so that the composition does not fully exert the function of ganoderma lucidum spore oil in the formula for protecting the gastric mucosa, and the patent does not provide the delay effect of the composition on symptoms caused by ethanol.
The patent 'an oil mixture capable of dispelling effects of alcohol' (CN 103211856A) is prepared by 50-60% of soybean oil, 10-15% of deer oil, 10-15% of ganoderma lucidum spore oil and 10-20% of rapeseed oil according to a certain proportion, wherein the compound combination causes the active ingredients which really exert the effects to be undefined; the patent only provides a retarding effect of the mixture on the symptoms caused by ethanol, and does not provide a pharmacological effect of the mixture on the gastric mucosa.
The production process of the equipment used in the conventional supercritical extraction is generally that supercritical extraction is carried out in an extraction kettle I1-1, switch valves V1 and V2 are designed on the extraction kettle I to separate raw materials from target products, the target products and impurities are mixed with supercritical fluid to reach a separation kettle I2-1, the solubility of the target products and a part of impurities in the supercritical fluid is reduced under specific pressure and temperature, the target products and a part of impurities are separated and settled to the bottom of the separation kettle I2-1, the separation kettle I is provided with a trimming valve F1 and a collecting valve C1, other impurities are brought to the separation kettle III 2-3 by the supercritical fluid, the supercritical fluid becomes gas under specific pressure and temperature, the residual impurities are separated and settled to the bottom of the separation kettle III, and the separation kettle III is provided with a trimming valve F2 and a collecting valve C3. After passing through the switch valve V7, the gaseous fluid is converted into liquid state through the heat exchanger II 3-2 under certain pressure and temperature and returns to the storage tank 4, and the liquid fluid in the storage tank is converted into supercritical fluid through the switch valve V8, the high-pressure pump 5, the switch valve V6 and the heat exchanger I3-1 and enters the extraction kettle I for supercritical extraction again.
The conventional supercritical extraction equipment is only suitable for single extraction, if the crude product in the separation kettle I is subjected to secondary extraction, the extraction kettle I needs to be opened, the crude product in the separation kettle I is poured, the continuity of production is not facilitated, the operation time is prolonged, and the crude product in the separation kettle I is easily oxidized by air or polluted.
Disclosure of Invention
The invention aims to overcome the defects of the ganoderma lucidum spore oil product and provide ganoderma lucidum spore oil with a protective effect on gastric mucosa and a preparation method thereof.
The technical scheme adopted by the invention is to prepare the ganoderma lucidum spore oil with a protective effect on gastric mucosa, and the key point is that the ganoderma lucidum spore oil is obtained by extracting ganoderma lucidum spore powder by a supercritical carbon dioxide double extraction technology, the acid value of the ganoderma lucidum spore oil is less than or equal to 2KOH (mg/g), and the peroxide value is less than or equal to 0.1%.
Ganoderma spore oil can delay symptoms such as slow action, uncoordinated limb movement, deepening of breath, and slow frequency caused by ethanol (0.1 mL/10 g) for 20min; ethanol (0.1 mL/10 g) with the ganoderma lucidum spore oil capable of being remarkably reduced causes gastric mucosal injuries such as gastric bleeding or ulcer; the Ganoderma spore oil can remarkably reduce gastric mucosal injury such as gastric hemorrhage or ulcer caused by antiinflammatory pain (40 mg/kg).
The supercritical carbon dioxide double extraction technology refers to: extracting Ganoderma spore powder by supercritical carbon dioxide extraction to obtain Ganoderma spore crude oil, and purifying the Ganoderma spore crude oil by supercritical carbon dioxide extraction to obtain Ganoderma spore oil.
The invention creatively carries out supercritical carbon dioxide double extraction on the wall-broken ganoderma lucidum spore powder, and the wall-broken ganoderma lucidum spore powder can not completely separate plasticizers, free carboxylic acid, peroxide, other impurities and the like in ganoderma lucidum spore oil only by one-time supercritical carbon dioxide extraction. The obtained Ganoderma spore oil with active ingredients contains a certain amount of free carboxylic acid, peroxide, pigment and other impurities, which results in relatively high acid value and peroxide value of Ganoderma spore oil, plasticizer residue is often found in spore oil, and pharmacological activity is affected. If the wall-broken ganoderma lucidum spore powder is directly extracted by using the purification process parameters, the ganoderma lucidum spore oil is low in yield and high in cost.
The supercritical double extraction purification separation equipment for producing the ganoderma lucidum spore oil with the gastric mucosa protection effect comprises an extraction kettle I, a separation kettle III, a heat exchanger I, a heat exchanger II, a storage tank, a high-pressure pump, a fine adjustment valve F, a collection valve C, a switch valve V and a control system, wherein the control system controls the working states of all components.
The preparation process of the ganoderma lucidum spore oil comprises the following steps: collecting mature ganoderma lucidum spores, collecting the ganoderma lucidum spores into powder, sieving to remove impurities, drying until the moisture is below 3%, breaking the wall, then taking a certain weight of wall-broken ganoderma lucidum spore powder, putting the wall-broken ganoderma lucidum spore powder into an extraction kettle I of a supercritical extraction device, sealing, introducing supercritical carbon dioxide, and performing first supercritical extraction: extracting kettle I with pressure of 20-30MPa, extracting kettle I with temperature of 40-50 ℃, separating kettle I with pressure of 8MPa, separating kettle I with temperature of 40-50 ℃, separating kettle III with pressure of 5-6MPa, separating kettle III with temperature of 40-50 ℃, flow rate of 550-650L/h, extracting time of 5-7h, obtaining ganoderma lucidum spore crude oil from separating kettle I, recycling ganoderma lucidum spore crude oil, conveying to extracting kettle II, introducing supercritical carbon dioxide, and performing second supercritical extraction: extracting kettle II with pressure of 20-30MPa, extracting kettle II with temperature of 40-50 ℃, separating kettle II with pressure of 10-15MPa, separating kettle II with temperature of 40-50 ℃, separating kettle III with pressure of 5-6MPa, separating kettle III with temperature of 40-50 ℃, flow rate of 550-650L/h, extracting time of 5-7h, and obtaining ganoderma lucidum spore oil from separating kettle II.
The invention improves on the basis of the prior conventional supercritical extraction equipment, adds the extraction kettle II, the recovery pipeline and the separation kettle II, connects the separation kettle I and the extraction kettle II through the recovery pipeline, and leads the obtained product in the separation kettle I to directly enter the extraction kettle II through the recovery pipeline, thereby being beneficial to automatic production, saving time and high efficiency, effectively preventing the obtained product in the first extraction separation kettle I from being oxidized or polluted in the moving process, and saving cost and occupied space compared with two sets of independent supercritical extraction equipment because the extraction kettle I and the extraction kettle II share the separation kettle III, the heat exchanger, the fluid storage tank, the high-pressure pump, the pipelines and the valves communicated with each other.
The method comprises the following steps of: the extraction kettle I is connected with a communicating pipeline through a switch valve V2, the extraction kettle II is connected with a separating kettle I through a fine tuning valve F1 and the separating kettle II through a fine tuning valve F4, a control system controls the switch valves V1, V2 and the fine tuning valves F1 and F2 to be simultaneously opened, at the moment, the switch valves V4, V3 and the fine tuning valves F3 and F4 are in a closed state, otherwise, the switch valves V4, V3 and the fine tuning valves F4 and F3 are simultaneously opened, and the switch valves V1, V2 and the fine tuning valves F1 and F2 are controlled to be in a closed state.
The extraction kettle I and the extraction kettle II are discharged and share a communication pipeline, the extraction kettle I and the extraction kettle II do not work simultaneously in the production process, when the extraction kettle I works, a valve related to the work of the extraction kettle II is closed, after the work of the extraction kettle I is completed, the working valve of the extraction kettle I is closed, the switch valve V5 is opened, the obtained product in the first extraction separation kettle I enters the extraction kettle II, and after the completion, the valve related to the extraction kettle II is opened, and the extraction kettle II enters the working state.
Better design: the extraction kettle I is connected with the extraction pipeline I through the switch valve V2 and is connected with the fine tuning valve F1 of the separation kettle I through the extraction pipeline I so as to be communicated with the separation kettle I, the extraction kettle II is connected with the extraction pipeline II through the switch valve V3 and is connected with the fine tuning valve F4 of the separation kettle II through the extraction pipeline II so as to be communicated with the separation kettle II, the switch valves V1, V2 and the fine tuning valves F1 and F2 are simultaneously opened or closed, and the switch valves V4, V3 and the fine tuning valves F3 and F4 are simultaneously opened or closed, so that the states of the extraction kettle I and the separation kettle II are controlled by a control system.
The pipelines for discharging the extraction kettle I and the extraction kettle II to the separation kettle are independently arranged, so that the extraction kettle I and the extraction kettle II can work simultaneously, time is saved, and industrial production is facilitated.
The pressure resistance of the extraction kettle I, the extraction kettle II, the fine adjustment valve F, the switch valve V and the pipeline is up to 50MPa; the pressure resistance of the separation kettle I, the separation kettle II, the separation kettle III and the collection valve C is up to 20MPa; the pressure resistance of the storage tank is up to 10MPa; the pressure of the high-pressure pump can reach 50MPa.
The ganoderma lucidum spore oil can be prepared into gastric mucosa oral preparation by adding auxiliary materials which are approved by medical science, pharmacy or food industry.
The gastric mucosa oral preparation can be used as food, health food or medicine.
When the ganoderma lucidum spore oil is used as a raw material of food, health-care food or medicine, the gastric mucosa oral preparation can have the effects of protecting gastric mucosa, preventing gastric mucosa injury ulcer and bleeding.
The gastric mucosa oral preparation comprises, but is not limited to, tablets, capsules, pills, granules, suspensions, dripping pills or oral liquid preparations.
The Ganoderma spore powder is a collection of spores of Karst of Polyporaceae fungus Ganoderma lucidum Ganoderma lucidum (Leys. Ex Fr.) recorded in the pharmacopoeia 2020 of the people's republic of China.
The technical scheme adopted by the invention adopts careful process design, and the experiment is repeated for a plurality of times, and adopts specific process parameters, so that the method has the beneficial effects that:
1. the supercritical carbon dioxide double extraction technology used in the invention comprises the following steps: extracting Ganoderma spore powder by supercritical carbon dioxide technology to obtain Ganoderma spore crude oil for the first time, and extracting and purifying Ganoderma spore crude oil for the second time to obtain Ganoderma spore oil enriched with active components with protective effect on gastric mucosa. The double extraction can overcome the defect that the supercritical carbon dioxide technology can not directly and accurately separate specific active ingredients in the ganoderma lucidum spore oil contained in the ganoderma lucidum spore powder, can accurately separate ganoderma lucidum spore crude oil, remove impurities and enrich active ingredients; the double extraction uses the same set of supercritical equipment, and compared with other equipment and technology such as supercritical and molecular distillation, the equipment cost can be effectively reduced, the process is simplified, and the time is saved; the supercritical carbon dioxide extraction technology is an extraction technology capable of passing through organic authentication, so that the ganoderma lucidum spore oil can be subjected to organic authentication.
2. The acid value of the ganoderma lucidum spore oil is less than or equal to 2KOH (mg/g), and the peroxide value is less than or equal to 0.1 percent; the quality is stable, the index is far lower than the specification of GB 2716 food safety national standard vegetable oil (acid value is less than or equal to 4KOH (mg/g), and peroxide value is less than or equal to 0.25 percent); at the same time, phthalate residues are not detected;
the invention uses unsaturated fatty acid as a marking component to screen pharmacological test samples, and the total content of unsaturated fatty acid in the ganoderma lucidum spore oil is found to be larger than that in ganoderma lucidum spore crude oil, and simultaneously, the ganoderma lucidum spore triple extract oil is obtained by using a supercritical triple extraction technology. The ganoderma lucidum spore oil has great potential in pharmacological activity and preparation of functional foods, health-care foods and medicines.
4. Pharmacological experiments further prove that the ganoderma lucidum spore oil can delay the occurrence time of symptoms such as slow action, uncoordinated limb movement, deepening of breathing, slow frequency and the like caused by ethanol (0.1 mL/10 g), and the delay time is 20min; ethanol (0.1 mL/10 g) with the ganoderma lucidum spore oil capable of being remarkably reduced causes gastric mucosal injuries such as gastric bleeding or ulcer; the Ganoderma spore oil can remarkably reduce gastric mucosal injury such as gastric hemorrhage or ulcer caused by antiinflammatory pain (40 mg/kg).
5. Compared with the conventional supercritical extraction equipment, the invention has the following advantages and beneficial effects: the invention can perform supercritical double extraction, purification and separation on line: the supercritical extraction capacity can be exerted during the first extraction, and the crude product with high yield is extracted; the waste liquid returns to another extraction kettle II through a recovery pipeline to carry out secondary extraction, and is accurately separated by using another separation kettle II, so that the high-purity accurate separation product is obtained while the yield is also achieved. Meanwhile, since the precisely separated product is not exposed to air for oxidation, the activity is higher than that of the crude product extracted at one time.
Drawings
FIG. 1 is a schematic diagram of a conventional supercritical apparatus
FIG. 2 is a schematic diagram of a supercritical double extraction purification separation apparatus according to example 1 of the present invention
FIG. 3 is a schematic view of a supercritical double extraction purification separation apparatus according to example 2 of the present invention, wherein: 1-1, extraction kettle I, 1-2, extraction kettle II, 2-1, separation kettle I, 2-2, separation kettle II, 2-3, separation kettle III, 3-1, heat exchanger I, 3-2, heat exchanger II, 4, storage tank, 5, high-pressure pump, 6, recovery pipeline, 7, extraction pipeline I, 8, extraction pipeline II, 9, communicating pipeline, F1-F4, fine tuning valve, C1-C3, collection valve, V1-V8, switch valve.
Detailed Description
The following examples further illustrate the invention but are not to be construed as limiting the invention and modifications or alternatives to the methods, steps or conditions of the invention are within the scope of the invention without departing from the spirit and nature of the invention.
A ganoderma lucidum spore oil with a protective effect on gastric mucosa is obtained by extracting ganoderma lucidum spore powder by a supercritical carbon dioxide double extraction technology, wherein the double extraction technology is to extract ganoderma lucidum spore powder by using the supercritical carbon dioxide extraction technology to obtain ganoderma lucidum spore crude oil, and the first extraction is; purifying the ganoderma lucidum spore crude oil by using a supercritical carbon dioxide extraction technology to obtain ganoderma lucidum spore oil, wherein the second extraction is performed;
the preparation process of the ganoderma lucidum spore oil comprises the following steps: collecting mature ganoderma lucidum spores, collecting the ganoderma lucidum spores into powder, sieving to remove impurities, drying until the moisture is below 3%, breaking the wall, then taking a certain weight of wall-broken ganoderma lucidum spore powder, putting the wall-broken ganoderma lucidum spore powder into an extraction kettle I of a supercritical extraction device, sealing, introducing supercritical carbon dioxide, and performing first supercritical extraction: extracting kettle I with pressure of 20-30MPa, extracting kettle I with temperature of 40-50 ℃, separating kettle I with pressure of 8MPa, separating kettle I with temperature of 40-50 ℃, separating kettle III with pressure of 5-6MPa, separating kettle III with temperature of 40-50 ℃, flow rate of 550-650L/h, extracting time of 5-7h, obtaining ganoderma lucidum spore crude oil from separating kettle I, recycling ganoderma lucidum spore crude oil, conveying to extracting kettle II, introducing supercritical carbon dioxide, and performing second supercritical extraction: extracting kettle II with pressure of 20-30MPa, extracting kettle II with temperature of 40-50 ℃, separating kettle II with pressure of 10-15MPa, separating kettle II with temperature of 40-50 ℃, separating kettle III with pressure of 5-6MPa, separating kettle III with temperature of 40-50 ℃ and flow rate of 550-650L/h, extracting time of 5-7h, and obtaining ganoderma lucidum spore oil from separating kettle II.
The acid value detection method of the ganoderma lucidum spore crude oil and the ganoderma lucidum spore oil is the determination of the acid value in GB 5009.229 food safety national standard food;
the detection method of the peroxide value of the ganoderma lucidum spore crude oil and the ganoderma lucidum spore oil is the measurement of the peroxide value in GB 5009.227 food safety national standard food.
The phthalate method of the ganoderma lucidum spore crude oil and the ganoderma lucidum spore oil is the determination of phthalate in GB 5009.271 food safety national standard food.
Supercritical double extraction purification separation equipment for preparing ganoderma lucidum spore oil with gastric mucosa protecting effect
Example 1
As shown in figure 2, the extraction, purification and separation equipment is improved on the basis of conventional supercritical equipment, and additional extraction kettles II 1-2, separation kettles II 2-2, a recovery pipeline 6, a corresponding fine tuning valve F, a collection valve C and a switch valve V are added, so that the whole equipment can perform extraction, purification and separation on line at the same time, and high-yield and high-purity accurate separation products are obtained.
The supercritical double extraction purification separation device comprises an extraction kettle I1-1, an extraction kettle II 1-2, a recovery pipeline 6, a separation kettle II 2-2, a separation kettle I2-1, a separation kettle III 2-3, a heat exchanger I3-1, a heat exchanger II 3-2, a storage tank 4, a high pressure pump 5, a communicating pipeline 9, a fine tuning valve F, a collecting valve C, a switching valve V and a control system, wherein the working states of all components are controlled by the control system, and the extraction kettle I and the extraction kettle II share the equipment between the separation kettle III, the heat exchanger II, a storage tank and the high pressure pump and the heat exchanger I and a connecting channel of the equipment.
The inlet of the extraction kettle I is connected with a switch valve V1, and the outlet is connected with a switch valve V2;
the inlet of the extraction kettle II is connected with a switch valve V4, and the outlet is connected with a switch valve V3;
the separation kettle I is connected with a fine tuning valve F1, a pipeline is communicated with the separation kettle III, the pipeline is connected with a fine tuning valve F2, a switch valve V5 and a recovery pipeline 6 are connected to the extraction kettle II, the bottom of the separation kettle I is connected with a collection valve C1, and crude products separated by the first extraction can be discharged from the collection valve C1 of the separation kettle I for detection and the like;
the separation kettle II is connected with a fine tuning valve F4; a pipeline is communicated with the separation kettle III, and a fine tuning valve F3 is connected in the pipeline; the bottom is connected with a collecting valve C2, and the precise separation product of the second extraction and purification is discharged from the collecting valve C2 of the separation kettle II;
the separation kettle III is communicated with the separation kettle I and the separation kettle II, a collection valve C3 is connected, waste is discharged from the collection valve C3 of the separation kettle III, a pipeline is communicated with the heat exchanger II, a switch valve V7 is connected in the pipeline, a channel from the separation kettle III, the heat exchanger II, the storage tank 4 and the high-pressure pump 5 to the heat exchanger I is the same as the prior art, and the heat exchanger II is connected with the storage tank 4; the storage tank is connected with the high-pressure pump through a switch valve V8; the high-pressure pump is connected with the heat exchanger I through a switch valve V6.
Fluid enters the extraction kettle I through the switch valve V1, enters the extraction kettle II through the valve V4, the recovery pipeline is connected between the separation kettle I and the extraction kettle II, the extraction kettle II is connected with the fine tuning valve F4 of the separation kettle II through the switch valve V3 so as to be communicated with the separation kettle II, the separation kettle II is connected with the separation kettle III through the fine tuning valve F3, and the separation kettle I and the separation kettle II are respectively connected with the separation kettle III.
The extraction kettle I is connected with the communicating pipeline 9 through the switch valve V2, the extraction kettle II is connected with the separation kettle I through the fine adjustment valve F1 and the separation kettle II through the fine adjustment valve F4, the control system controls the switch valves V1, V2 and the fine adjustment valves F1 and F2 to be simultaneously opened, at the moment, the switch valves V4, V3 and the fine adjustment valves F3 and F4 are in a closed state, otherwise, the switch valves V4, V3 and the fine adjustment valves F4 and F3 are simultaneously opened, and the switch valves V1, V2 and the fine adjustment valves F1 and F2 are controlled to be in a closed state.
The extraction kettle I and the extraction kettle II are discharged and share a communication pipeline, the extraction kettle I and the extraction kettle II do not work simultaneously in the production process, when the extraction kettle I works, a valve related to the work of the extraction kettle II is closed, after the work of the extraction kettle I is completed, the valve related to the work of the extraction kettle I is closed, a switch valve V5 is opened, a product in the first extraction separation kettle I enters the extraction kettle II, and after the completion, the valve related to the extraction kettle II is opened, and the extraction kettle II enters a working state.
The pressure resistance of the extraction kettle I, the extraction kettle II, the fine adjustment valve F, the switch valve V and the pipeline is up to 50MPa; the pressure resistance of the separation kettle I, the separation kettle II, the separation kettle III and the collection valve C is up to 20MPa; the pressure resistance of the storage tank is up to 10MPa; the pressure of the high-pressure pump can reach 50MPa. The remaining non-described parts are identical to the prior art.
A method for extracting a product by utilizing supercritical double extraction, purification and separation equipment comprises the following operation steps: preparation of ganoderma lucidum spore oil: collecting mature ganoderma lucidum spores, collecting the ganoderma lucidum spores into powder, sieving to remove impurities, drying until the moisture is less than 3%, breaking the wall, taking 100kg, recording the raw material I, putting the ganoderma lucidum spores into an extraction kettle of a supercritical extraction device, sealing, opening switch valves V1, V2, V6, V7 and V8, finely adjusting valves F1 and F2, introducing supercritical carbon dioxide, and performing supercritical extraction: extracting kettle I pressure 20MPa, extracting kettle I temperature 50 ℃, separating kettle I pressure 8MPa, separating kettle I temperature 50 ℃, separating kettle III pressure 5MPa, separating kettle III temperature 50 ℃, flow 650L/h, extracting time 7h, closing switch valves V1, V2, fine tuning valves F1 and F2, obtaining ganoderma lucidum spore crude oil I from separating kettle I, opening switch valve V5, recycling ganoderma lucidum spore crude oil I and conveying to extracting kettle II, sealing, closing switch valve V5, opening switch valves V3, V4, fine tuning valves F3 and F4, introducing supercritical carbon dioxide, and performing second supercritical extraction: extracting kettle II with pressure of 30MPa, extracting kettle II with temperature of 40 ℃, separating kettle II with pressure of 10MPa, separating kettle II with temperature of 40 ℃, separating kettle III with pressure of 6MPa, separating kettle III with temperature of 40 ℃, flow rate of 550L/h, extracting time of 5h, opening collecting valve C2, obtaining Ganoderma spore oil I from separating kettle II with weight of 18.0kg,
example 2
As shown in figure 3, the extraction, purification and separation equipment is improved on the basis of conventional supercritical equipment, and additional extraction kettles II, separation kettles II, recovery pipelines, corresponding fine tuning valves F, collection valves C and switching valves V are added, so that the whole equipment can perform extraction, purification and separation on line at the same time, and high-yield and high-purity accurate separation products are obtained.
The supercritical double extraction purification separation equipment comprises an extraction kettle I, an extraction kettle II, a recovery pipeline, a separation kettle II, a separation kettle I, a separation kettle III, a heat exchanger I, a heat exchanger II, a storage tank, a high-pressure pump, an extraction pipeline I, an extraction pipeline II, a fine adjustment valve F, a collection valve C, a switching valve V and a control system, wherein the control system controls the working states of all components, the extraction kettle I and the extraction kettle II share the existing extraction purification separation equipment, and the separation kettle III, the heat exchanger II, the storage tank, equipment between the high-pressure pump and the heat exchanger I and a connecting channel of the equipment.
The extraction kettle I is connected with the extraction pipeline I7 through the switch valve V2 and is connected with the fine tuning valve F1 of the separation kettle I through the extraction pipeline I so as to be communicated with the separation kettle I, the extraction kettle II is connected with the extraction pipeline II 8 through the switch valve V3 and is connected with the fine tuning valve F4 of the separation kettle II through the extraction pipeline II so as to be communicated with the separation kettle II, the switch valves V1, V2 and the fine tuning valves F1 and F2 are simultaneously opened or closed, and the switch valves V4, V3 and the fine tuning valves F3 and F4 are simultaneously opened or closed, and the state of the extraction kettle I is controlled by a control system. The remaining undescribed portions are the same as in example 1.
A method for extracting a product by utilizing supercritical double extraction, purification and separation equipment comprises the following operation steps of: and after the previous extraction is finished, all valves are closed, the switch valve V5 is opened to recycle and convey the crude product in the separation kettle I to the extraction kettle II, the extraction kettle II is sealed, and the switch valve V5 is closed. Taking a certain amount of raw materials, putting the raw materials into an extraction kettle I of a supercritical extraction device, sealing, opening switch valves V1, V2, V4, V3, V6, V7 and V8, fine adjusting valves F1, F2, F3 and F4, introducing supercritical carbon dioxide, and performing supercritical extraction: the extraction time is 5-7h, the pressure of the extraction kettle I is 20-30MPa, the temperature of the extraction kettle I is 40-50 ℃, the pressure of the separation kettle I is 8MPa, the temperature of the separation kettle I is 40-50 ℃, the pressure of the separation kettle III is 5-6MPa, and the temperature of the separation kettle III is 40-50 ℃; at this time, the extraction kettle II carries out a second supercritical extraction on the crude product collected by the previous separation kettle I: the extraction time is 5-7h, the pressure of the extraction kettle II is 20-30MPa, the temperature of the extraction kettle II is 40-50 ℃, the pressure of the separation kettle II is 10-15MPa, the temperature of the separation kettle II is 40-50 ℃, and the collection valve C2 is opened to obtain the precise separation product from the separation kettle II. The pressure of the separation kettle III is 5-6MPa, the temperature of the separation kettle III is 40-50 ℃, and the flow is 1100-1300L/h. Since the time of the two extractions may be different, the respective switches of the two extraction systems may be controlled by the control system. If the extraction kettle I is ended, the switch valve V1 and the switch valve V2 can be closed first. Depressurizing the extraction kettle I, taking out the extracted raw materials, and putting new raw materials into the extraction kettle I; if the extraction kettle II is finished, the switch valves V4 and V3 can be closed, the collection valve C2 is opened, and the precise separation product is obtained from the separation kettle II. And (3) depressurizing the extraction kettle II, opening a switch valve V5 to recycle and convey the crude product in the separation kettle I into the extraction kettle II, sealing, closing the switch valve V5, and performing second supercritical extraction. The collecting valve C3 can be opened during supercritical extraction, and the waste is discharged from the collecting valve C3 of the separating kettle III, so that continuous production is performed.
A method for extracting a product by utilizing supercritical double extraction, purification and separation equipment comprises the following operation steps: harvesting mature ganoderma lucidum spores, collecting the ganoderma lucidum spores into powder, sieving to remove impurities, drying until the moisture is below 3%, breaking the wall, taking 100kg, recording raw material II, and using the device for the first time, wherein the extraction kettle I works, and the extraction kettle II does not work. Putting a raw material II into an extraction kettle of a supercritical extraction device, sealing, opening switch valves V1, V2, V6, V7 and V8, fine adjusting valves F1 and F2, introducing supercritical carbon dioxide, and performing supercritical extraction: extracting kettle I pressure 25MPa, extracting kettle I temperature 45 ℃, separating kettle I pressure 8MPa, separating kettle I temperature 45 ℃, separating kettle III pressure 6MPa, separating kettle III temperature 45 ℃, flow 600L/h, extracting time 6h, obtaining ganoderma lucidum spore crude oil II from separating kettle I, closing V1, V2, fine tuning valves F1 and F2, opening switch valve V5, recovering and conveying ganoderma lucidum spore crude oil II into extracting kettle II, sealing, closing switch valve V5, opening switch valves V3 and V4, fine tuning valves F3 and F4, introducing supercritical carbon dioxide, extracting kettle II for carrying out second supercritical extraction of ganoderma lucidum spore crude oil II: extracting time is 6h, the pressure of the extraction kettle II is 25MPa, the temperature of the extraction kettle II is 45 ℃, the pressure of the separation kettle II is 13MPa, the temperature of the separation kettle II and the separation kettle is 45 ℃, after extraction is finished, a collecting valve C2 is opened, and ganoderma lucidum spore oil II is obtained from the separation kettle II by about 16.0 kg. And (3) reducing the pressure of the extraction kettle I while extracting the extraction kettle II, discharging the extracted raw material II, taking 100kg of the raw material III, recording the raw material III, and putting the raw material III into the extraction kettle I, wherein the extraction kettle I performs first extraction of the raw material III at the moment: the extraction time is 5h, the pressure of the extraction kettle I is 30MPa, the temperature of the extraction kettle I is 40 ℃, the pressure of the separation kettle I is 8MPa, and the temperature of the separation kettle I is 40 ℃. After the second extraction of the raw material II and the first extraction of the raw material III are finished, the ganoderma lucidum spore oil II obtained by taking out from the separation kettle II is about 16.0kg, then the switch valves V3 and V4 are closed, the extraction kettle II is depressurized, the switch valve V5 is opened, and the ganoderma lucidum spore crude oil III extracted from the raw material III is recovered and conveyed into the extraction kettle II for the second extraction of the raw material III: the extraction time is 7h, the pressure of the extraction kettle II is 20MPa, the temperature of the extraction kettle II is 50 ℃, the pressure of the separation kettle II is 15MPa, the temperature of the separation kettle II is 50 ℃, the pressure of the separation kettle III is 6MPa, the temperature of the separation kettle III is 40 ℃, the flow rate is 1300L/h, a collection valve C2 is opened, and about 15.7kg of ganoderma lucidum spore oil III is obtained from the separation kettle II. While continuing to extract … … of the raw material IV
Detecting the obtained product
After each first extraction of examples 1 and 2 was completed, a collection valve C1 was opened, a small amount of crude oil I, II and III of ganoderma lucidum spores was taken from a separation vessel I, after each second extraction of examples 1 and 2 was completed, a collection valve C2 was opened, a small amount of crude oil I, II and III of ganoderma lucidum spores was taken from a separation vessel II, acid value and peroxide value were detected, the detection results are shown in Table 1, the crude oil I, II and III of ganoderma lucidum spores of examples 1-2 were mixed, the crude oil I, II and III of ganoderma lucidum spores were mixed, phthalate content was detected, the detection results are shown in Table 2, and the mixture was placed in a sealed vessel and placed in an environment of 37℃for 3 months, acid value and peroxide value were detected monthly, and the detection results are shown in Table 4
TABLE 1 acid value and peroxide value of Ganoderma lucidum spore oil
| Sample of | Acid value KOH (mg/g) | Peroxide value% |
| Glossy ganoderma spore crude oil I | 3.07 | 0.1363 |
| Ganoderma lucidum spore oil I | 1.96 | 0.0882 |
| Glossy ganoderma spore crude oil II | 3.11 | 0.1353 |
| Glossy ganoderma spore oil II | 1.74 | 0.0836 |
| Glossy ganoderma spore crude oil III | 3.27 | 0.1486 |
| Glossy ganoderma spore oil III | 1.53 | 0.0545 |
TABLE 2 phthalate content of Ganoderma spore oil
TABLE 3 phthalate names and abbreviations
| Sequence number | Chinese name | English name | Abbreviations (abbreviations) | CAS number |
| 1 | Di-n-butyl phthalate | Dibutyl phthalate | DBP | 84-74-2 |
| 2 | Di (2-ethyl) hexyl phthalate | Bis(2-ethylhexyl)phthalate | DEHP | 117-81-7 |
TABLE 4 acid value and peroxide value stability of Ganoderma lucidum spore oil
Animal test
Protection of ganoderma lucidum spore oil on gastric mucosa and time effect of delaying occurrence of ethanol effect
Test animals
120 SPF-grade ICR mice, male, were purchased from Shanghai Laek laboratory animal Co., ltd (production license number: SCXK (Shanghai) 2016-0003). The feed is fed into SPF grade animal feeding room (using qualification: SYXK 2014-005), room temperature (22+ -2), humidity (60+ -5)%, and fed with standard pellet feed, free drinking water and ingestion.
Main drugs and reagents
Ganoderma lucidum spore oil (a mixed sample of Ganoderma lucidum spore oils I, II, and III of examples 1 and 2) was provided by Fujian Xianzhu Biotechnology Co., ltd; omeprazole (lot number 060190533, european Italian pharmaceutical Co., ltd.); indomethacin (lot number: 1180801, beijing Red Lin pharmaceutical Co., ltd.).
Main instrument
BSA223S-CW type analytical balance (Sartorius Corp., germany); milli-Q ultra-pure water machine (Millipore Co., U.S.A.); BT224S electronic balance (Sidoris weighing device Co., ltd.)
Method
Basis for selection of dosage
According to the method described in pharmacological and traditional Chinese medicine pharmacological experiments, equivalent dose conversion between human and animals is carried out, and the calculation formula is as follows: animal equivalent dose (g/kg) =total daily dose (g)/60 kg× (human conversion factor/animal conversion factor). According to the clinical dose of ganoderma lucidum spore oil provided by the consignment unit, calculating the equivalent dose of the mice, setting the equivalent dose as a medium dose, wherein the equivalent dose is multiplied by 1/2 times as a low dose, and the equivalent dose is multiplied by 2 times as a high dose.
Grouping
Mice were divided into 6 groups, each: blank group, model group (ethanol and indomethacin group), omeprazole group, ganoderma lucidum spore oil low dose group, ganoderma lucidum spore oil medium dose group, ganoderma lucidum spore oil high dose group, 20 groups each.
Modeling and administration
Omeprazole group: 4mg/kg, 1 administration by lavage per day; low, medium and high dosage groups of ganoderma lucidum spore oil: the administration doses are respectively 0.2 g/kg, 0.4 g/kg, the blank control group and the model group are respectively given with equal volumes of physiological saline, the normal saline is administrated by intragastric administration for 1 time every day, after continuous administration for 7d, the fasted period is 12 hours, 10 mice are randomly selected for each group to be administrated by intragastric administration of ethanol (0.1 mL/10 g), and the sample collection is carried out after 1.5 hours; the remaining mice in each group were given indomethacin (40 mg/kg) and given intragastrically, and 3 hours later were subjected to sample collection.
General Condition observations
During the experiment, the general conditions of the mice, such as mental state, physical quality, hair color, activity, response sensitivity, death status and the like are recorded; body weights were weighed 3 times a week at the same time and recorded.
Sample collection and observation
The cervical dislocation of the mice is killed, the stomach is taken out by laparotomy, the pylorus and the cardia are ligated, 2-3mL of 4% paraformaldehyde solution is injected from the joint of the duodenum and the pylorus, after the mice are fixed for 20min, the mice are sheared along the greater curvature of the stomach, gastric contents are washed, gastric mucosa is unfolded, and the mice are sucked dry by filter paper, so that the damage degree of the gastric mucosa is observed.
Evaluation method and scoring criteria
The maximum length and width of the gastrorrhagia or ulcer were measured with a vernier caliper, and the maximum width of the bleeding or ulcer was used as an index of injury. The scoring criteria are shown in Table 5.
TABLE 5 scoring criteria for acute gastric mucosal lesion model
Note that: the length and width are measured in terms of maximum diameter.
And (3) observing the indexes: the degree of gastric mucosal lesion in each experimental group was expressed as a lesion occurrence rate (%) and a lesion inhibition rate (%). Incidence of injury (%) = number of mice in a group with bleeding or ulceration/number of mice in the group x 100%; injury inhibition (%) = (a-B)/a×100% (A, B is the injury integral of model and drug groups, respectively)
Statistical analysis
Test data are expressed as mean ± standard deviation (x±s), and single-factor analysis of variance is performed using SPSS 20.0 statistical software. The difference of P <0.01 is statistically significant.
Results
General cases
The mice in each group had no abnormality in the administration process. After the mice are given with ethanol, the model group and the omeprazole group begin to have symptoms of slow movement, uncoordinated limb movement, deepened respiration, slow frequency and the like after 10 minutes; the mice given the ganoderma lucidum spore oil are subjected to symptoms of slow movement, uncoordinated limb movement, deepening of breath, slow frequency and the like after 30 minutes, and the time for the symptoms is prolonged with the increase of the administration dosage. Mice given indomethacin had reduced voluntary activity and no difference between groups. The mice in the blank group treated with physiological saline had normal behavioural activities, and the symptoms were not observed.
Gastric bleeding or ulcer
The gastrorrhagia or ulcer of each group of mice was observed as follows: the blank group has no gastrorrhagia or ulcer, and the mucous membrane is complete. For acute gastric ulcer caused by ethanol: the model group (ethanol group) can be seen with a large number of streak and plaque bleeding; the omeprazole group can see a great deal of strip bleeding, and the plaque bleeding degree is slightly lighter than that of the ethanol group; the ganoderma lucidum spore oil low dose group only has few tiny bleeding points, and has no strip bleeding and sheet mucosa bleeding ulcer; the dosage group of ganoderma lucidum spore oil only has 1 tiny bleeding point, and no strip bleeding and plaque bleeding; the high dosage group of Ganoderma spore oil has no gastrorrhagia or ulcer, and the gastric mucosa is substantially different from the blank group. For gastric ulcer caused by indomethacin: the model group (anti-inflammatory pain group) can be seen to have a large number of strip ulcers and circular ulcer surfaces, a concave center, a lack of mucous membrane, extremely thin stomach wall and even gastric perforation; the omeprazole group can see a large number of strip ulcers and circular ulcer surfaces, the center is concave, mucous membranes are absent, and the stomach wall is slightly thicker than the model group; the ganoderma lucidum spore oil low dose group has few punctiform ulcer surfaces and strip ulcers, and the thickness of the stomach wall is slightly thinner than that of the blank group; the dosage group of ganoderma lucidum spore oil has few punctiform ulcer surfaces, 1 case of ganoderma lucidum spore oil has strip ulcers, and the thickness of the stomach wall is basically the same as that of the blank group; the high dosage group of Ganoderma spore oil has only a few punctate ulcer surfaces, and the thickness of stomach wall is basically the same as that of blank group.
Incidence of injury, injury index and injury inhibition rate
The gastric injury score results are shown in Table 6, and the gastric injury incidence, injury index and injury inhibition rate are shown in Table 7. Compared with a model group, the gastric mucosa injury (P < 0.01) such as gastric bleeding or ulcer can be obviously reduced by preventive administration of the ganoderma lucidum spore oil, wherein the injury incidence rate of the ganoderma lucidum spore oil group is obviously reduced (P < 0.01), and the injury inhibition rate of the ganoderma lucidum spore oil group is obviously improved (P < 0.01).
Table 6 gastric injury scoring results (x±s, n=10) for each group of mice
| Ethanol | Anti-inflammatory pain | |
| Blank group | 0 | 0 |
| Model group | 10.80±2.49 ## | 5.20±0.45 ## |
| Omeprazole group | 8.00±1.41 | 3.40±0.89 ** |
| Low dosage set of ganoderma lucidum spore oil | 0.40±0.55 ** | 0.80±1.10 ** |
| Dosage group in ganoderma lucidum spore oil | 0.20±0.45 ** | 0.40±0.89 ** |
| High dosage set of ganoderma lucidum spore oil | 0±0 ** | 0.20±0.45 ** |
Note that: in comparison with the blank set of the cells, ## P<0.01; in comparison with the set of models, ** P<0.01。
table 7 incidence of gastric injury, injury index and injury inhibition rate (x±s, n=10) for each group of mice
Note that: in comparison with the blank set of the cells, ## P<0.01; in comparison with the set of models, ** P<0.01。
summary
The experimental result shows that the administration of absolute ethyl alcohol or anti-inflammatory pain and gastric lavage to mice can cause serious gastric ulcer, and the administration of ganoderma lucidum spore oil can effectively inhibit the occurrence of gastric ulcer caused by absolute ethyl alcohol and anti-inflammatory pain of mice, and has remarkable effect on acute gastric ulcer caused by absolute ethyl alcohol.
Claims (5)
1. A preparation method of ganoderma lucidum spore oil with a protective effect on gastric mucosa is characterized in that ganoderma lucidum spore oil is obtained by extracting ganoderma lucidum spore powder by a supercritical carbon dioxide double extraction technology, the acid value of the ganoderma lucidum spore oil is less than or equal to 2KOH mg/g, and the peroxide value is less than or equal to 0.1%; the supercritical carbon dioxide double extraction technology refers to: extracting ganoderma lucidum spore powder by using a supercritical carbon dioxide extraction technology to obtain ganoderma lucidum spore crude oil in the first extraction, and purifying the ganoderma lucidum spore crude oil by using the supercritical carbon dioxide extraction technology to obtain ganoderma lucidum spore oil in the second extraction; the preparation process of the ganoderma lucidum spore oil comprises the following steps: collecting mature Ganoderma spore, collecting into powder, sieving to remove impurities, oven drying until water content is below 3%, breaking wall, collecting wall-broken Ganoderma spore powder, placing into extraction kettle I of supercritical extraction device, sealing, introducing supercritical carbon dioxide, and performing first supercritical extraction: extracting kettle I with pressure of 20-30MPa, extracting kettle I with temperature of 40-50 ℃, separating kettle I with pressure of 8MPa, separating kettle I with temperature of 40-50 ℃, separating kettle III with pressure of 5-6MPa, separating kettle III with temperature of 40-50 ℃, flow rate of 550-650L/h, extracting time of 5-7h, obtaining ganoderma lucidum spore crude oil from separating kettle I, recycling ganoderma lucidum spore crude oil, conveying to extracting kettle II, introducing supercritical carbon dioxide, and performing second supercritical extraction: extracting kettle II with pressure of 20-30MPa, extracting kettle II with temperature of 40-50 ℃, separating kettle II with pressure of 10-15MPa, separating kettle II with temperature of 40-50 ℃, separating kettle III with pressure of 5-6MPa, separating kettle III with temperature of 40-50 ℃, flow rate of 550-650L/h, extracting time of 5-7h, obtaining ganoderma lucidum spore oil from separating kettle II; wherein, the supercritical extraction device of the ganoderma lucidum spore oil comprises: the device comprises an extraction kettle I (1-1), a separation kettle I (2-1), a separation kettle III (2-3), a heat exchanger I (3-1), a heat exchanger II (3-2), a storage tank (4), a high-pressure pump (5), a fine adjustment valve F, a collection valve C, a switch valve V and a control system, wherein the control system controls the working states of all components, the device also comprises the extraction kettle II (1-2), a recovery pipeline (6) and the separation kettle II (2-2), the extraction kettle I (1-1) and the extraction kettle II (1-2) share fluid to enter the pipeline, the fluid enters the extraction kettle I through the switch valve V1 and enters the extraction kettle II through V4, the recovery pipeline (6) is connected between the separation kettle I (2-1) and the extraction kettle II (1-2), the extraction kettle II (1-2) is connected with the fine adjustment valve F4 of the separation kettle II (2-2) through the switch valve V3 so as to be communicated with the separation kettle II (2-2), and the separation kettle I (2-1) is respectively connected with the separation kettle II (2-3) through the fine adjustment valve F3; the pressure resistance of the extraction kettle I (1-1), the extraction kettle II (1-2), the fine adjustment valve F, the switch valve V and the pipeline is up to 50MPa; the pressure resistance of the separation kettle I (2-1), the separation kettle II (2-2), the separation kettle III (2-3) and the collecting valve C is up to 20MPa; the pressure resistance of the storage tank (4) is up to 10MPa; the pressure of the high-pressure pump (5) can reach 50MPa.
2. The method for preparing ganoderma lucidum spore oil with a protective effect on gastric mucosa according to claim 1, wherein the supercritical extraction device is characterized in that an extraction kettle I (1-1) is connected with a communicating pipeline (9) through a switch valve V2, an extraction kettle II (1-2) is connected with a separation kettle I (2-1) through a fine tuning valve F1 and a separation kettle II (2-2) through a fine tuning valve F4, a control system controls the switch valves V1 and V2 and the fine tuning valves F1 and F2 to be simultaneously opened, at the moment, the switch valves V4 and V3 and the fine tuning valves F3 and F4 are in a closed state, and conversely, the switch valves V4 and V3 and the fine tuning valves F4 and F3 are simultaneously opened, and the switch valves V1 and V2 and the fine tuning valves F1 and F2 are controlled to be in a closed state.
3. The method for preparing ganoderma lucidum spore oil with a protective effect on gastric mucosa according to claim 1, wherein an extraction kettle I (1-1) in the supercritical extraction device is connected with an extraction pipeline I (7) through a switch valve V2 and is connected with a fine tuning valve F1 of a separation kettle I through the extraction pipeline I (7) so as to be communicated with the separation kettle I (2-1), an extraction kettle II (1-2) is connected with an extraction pipeline II (8) through a switch valve V3 and is connected with a fine tuning valve F4 of the separation kettle II through the extraction pipeline II (8) so as to be communicated with the separation kettle II (2-2), the switch valves V1, V2 and the fine tuning valves F1 and F2 are simultaneously opened or closed, and the states of the switch valves V4, V3 and the fine tuning valves F4 are simultaneously opened or closed by a control system.
4. An oral preparation for gastric mucosa, which is characterized in that the oral preparation is prepared by adding auxiliary materials which are approved by medicine or pharmacy into ganoderma lucidum spore oil obtained by the preparation method of claim 1, wherein the content of ganoderma lucidum spore oil is 28-99 percent.
5. The oral preparation for gastric mucosa of claim 4, wherein the oral preparation for gastric mucosa is a tablet, capsule, pill, granule or oral liquid.
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