CN115125059A - Method for removing fat-soluble harmful ingredients in ganoderma lucidum spore oil - Google Patents
Method for removing fat-soluble harmful ingredients in ganoderma lucidum spore oil Download PDFInfo
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- CN115125059A CN115125059A CN202210675602.1A CN202210675602A CN115125059A CN 115125059 A CN115125059 A CN 115125059A CN 202210675602 A CN202210675602 A CN 202210675602A CN 115125059 A CN115125059 A CN 115125059A
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- ganoderma lucidum
- lucidum spore
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- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 1
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Classifications
-
- 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
-
- 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
-
- 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
-
- 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
- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Micro-Organisms Or Cultivation Processes Thereof (AREA)
Abstract
The invention discloses a method for removing fat-soluble harmful ingredients in ganoderma lucidum spore oil, which uses ethanol as an entrainer to carry out CO treatment on most of the fat-soluble harmful ingredients in raw material ganoderma lucidum spore powder without wall breaking 2 Performing supercritical extraction, eluting, breaking cell wall to obtain cell wall-broken Ganoderma spore powder, and recycling CO 2 Supercritical extraction to obtain Ganoderma spore oil without fat-soluble harmful components, with fragrant oil and long storage time. The method has the advantages of quick operation, low energy consumption, suitability for mass production and processing, effective removal of fat-soluble harmful ingredients, retention of effective active ingredients of the ganoderma lucidum spore powder, and consideration of safety, effectiveness and quality controllability of the ganoderma lucidum spore oil.
Description
Technical Field
The invention belongs to the technical field of medicine extraction, and particularly relates to a method for removing fat-soluble harmful ingredients in ganoderma lucidum spore oil.
Background
Ganoderma lucidum is recorded in the department of pharmacopoeia of the people's republic of China, 2020 edition, and is a dried fruiting body of Ganoderma lucidum (Leys. ex Fr.) Karst. or Ganoderma sinense Zhao, Xu et Zhang, a fungus of Polyporaceae. Has effects in invigorating qi, tranquilizing mind, relieving cough and asthma, and can be used for treating restlessness of heart-mind, insomnia, palpitation, cough and asthma due to lung deficiency, asthenia, short breath, and anorexia. The Ganoderma spore powder is tiny egg-shaped germ cells ejected from fold of Ganoderma during growth and maturation stage, and has all genetic active substances of Ganoderma. The Ganoderma spore powder is rich in pharmacological active components such as triterpenes, organic acids, polysaccharides, amino acids, and microelements, and has effects of resisting oxidation, protecting liver, enhancing immunity, assisting anti-tumor, and reducing blood lipid. The Ganoderma spore oil is prepared by drying Ganoderma spore powder, breaking cell wall, and supercritical CO extraction 2 The ganoderma lucidum spore powder is prepared by an extraction technology, enriches the triterpenes, sterols and unsaturated fatty acid components in the ganoderma lucidum spore powder, and has better effects on enhancing immunity and assisting anti-tumor. Along with the increasing demand of people for the ganoderma lucidum spore oil year by year, the quality safety problem of the ganoderma lucidum spore oil product also becomes a hot point of social attention. The quality problem of the ganoderma lucidum spore oil can be traced back to the raw material ganoderma lucidum spore powder and the intermediate product wall-broken ganoderma lucidum spore powder, and fat-soluble harmful components exist in the background. The main potential quality safety hazards are mainly free fatty acid, fat-soluble pesticide residue, plasticizer and mycotoxin, and the fat-soluble harmful components are dissolved in the extracted ganoderma lucidum spore oil, and the content of the components is concentrated to be 3-4 times of that of spore powder, so that the limit value is easily exceeded.
Ganoderma lucidum is generally cultivated in 5-9 months, in positive-value high-temperature rainy seasons, diseases and insect pests frequently occur, and the risk of pesticide residue exceeding the standard is caused if a chemical method is used for preventing insect pests. The prevention and treatment effect of the fat-soluble pesticide (the organic chlorine pesticide is hexachloro-cyclohexane, has strong fat solubility) is better than that of the water-soluble pesticide, but the fat-soluble pesticide is easy to absorb and accumulate in organisms and soil, and the residue of the fat-soluble pesticide is far greater than that of the water-soluble pesticide. Various plastic products are involved in the artificial cultivation, harvesting and processing processes of the lucid ganoderma, plasticizers (phthalic acid esters, PAEs) can be transferred into lucid ganoderma spore powder through plastic packages along with the passage of time, and although the PAEs have low acute toxicity, a large amount of plasticizers can bring chronic harm to the reproductive system, the immune system and the digestive system of a human body after long-term consumption. The ganoderma lucidum spore powder is easy to be detected to be aflatoxin B, and the ganoderma lucidum spore powder is easy to mildew after being collected and broken and exposed in humid air 1 、G 1 The aflatoxin belongs to a class I carcinogen and is a risk factor for the quality safety of the ganoderma lucidum spore oil. Under the conditions of high temperature and oxygen, unsaturated fatty acid is oxidized and degraded into volatile aldehyde, ketone, acid and other substances, so that rancidity is caused, and whether the peroxide value exceeds the standard or not directly influences the sensory quality of the ganoderma lucidum spore oil. The food with peroxide value exceeding the standard can promote cardiovascular and tumor diseases.
The quality safety problem of the ganoderma lucidum spore oil product not only relates to the benefit of consumers, but also relates to the healthy development of the edible fungus industry including ganoderma lucidum in China. The invention starts to control the ganoderma lucidum spore powder without wall breaking from the source, optimizes the production process flow, enhances the quality control of the product, reduces the occurrence of safety events of the ganoderma lucidum spore oil product and ensures the quality of the ganoderma lucidum spore oil product. Compared with the prior art, firstly, fat-soluble harmful ingredients including plasticizer are directly removed when the ganoderma lucidum spore oil is extracted, and the process flow is simplified; and secondly, the entrainer with specific concentration is adopted, so that the plasticizer residue and pollution in the ganoderma lucidum spore oil can be effectively and completely removed.
Disclosure of Invention
The invention aims to provide a method for removing fat-soluble harmful ingredients in ganoderma lucidum spore oil, which is suitable for large-scale industrial production.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
(1) adding 30-35% of water into the ganoderma lucidum spore powder without wall breaking, granulating, drying at 70-80 ℃ until the water content is lower than 5%, and sieving by a sieve of 10-20 meshes to obtain ganoderma lucidum spore powder particles without wall breaking;
(2) by mass concentration75 to 95 percent of ethanol is used as an entrainer, and the material-liquid ratio range is 2: 1-1: 2kg/L of a catalyst, CO 2 Supercritical extraction, wherein the extraction conditions are as follows: the pressure of the extraction kettle is 15-22 MPa, and the temperature is 45-60 ℃; the pressure of the separation kettle I is 6-10 MPa, and the temperature is 35-55 ℃; the pressure of the separation kettle II is 4-6 MPa, and the temperature is 20-40 ℃; CO 2 2 The flow rate is 400-800L/h, the extraction time is 1-2 h, an alcohol-oil mixture and spore powder particles are obtained, the spore powder particles are subjected to wall breaking to obtain wall-broken ganoderma lucidum spore powder, granulation is carried out to obtain wall-broken ganoderma lucidum spore powder particles, and the wall-broken ganoderma lucidum spore powder particles are sieved by a 10-mesh sieve;
(3) ethanol with the mass concentration of 75-95% is used as an entrainer, and the material-liquid ratio range is 1: 0.05-1: 0.15, carrying out CO 2 Supercritical extraction, wherein the extraction conditions are as follows: the pressure of the extraction kettle is 30-40 MPa, and the temperature is 50-70 ℃; the pressure of the separation kettle I is 10-12 MPa, and the temperature is 50-60 ℃; the pressure of the separation kettle II is 4-6 MPa, and the temperature is 30-40 ℃; CO 2 2 The flow rate is 700-900L/h, and the extraction time is 2.5-4.5 h, so that the defatted particles and the ganoderma lucidum spore oil are obtained.
Preferably, the feed-liquid ratio in the step (2) is 1-1.5: 1 to 1.5 (kg/L); most preferably, the feed-liquid ratio is 1: 1 (kg/L).
Preferably, in the step (2), the pressure of the extraction kettle is 18-22 MPa, and the temperature is 45-60 ℃. The pressure of the separation kettle I is 7-8 MPa, and the temperature is 40-50 ℃. The pressure of the separation kettle II is 4-5 MPa, and the temperature is 30-35 ℃. Most preferably CO in step (2) 2 Supercritical extraction: the pressure of the extraction kettle is 20MPa, and the temperature is 50 ℃; the pressure of the separation kettle I is 8MPa, and the temperature is 45 ℃; the pressure of the separation kettle II is 5MPa, and the temperature is 30 ℃; CO 2 2 The flow rate is 600L/h, and the extraction time is 1.5 h.
Preferably, the material-liquid ratio in the step (3) is in a range of 1: 0.1 (kg/L);
preference is given to CO in step (3) 2 Supercritical extraction: the pressure of the extraction kettle is 35-40 MPa, and the temperature is 60-65 ℃. The pressure of the separation kettle I is 10-12 MPa, and the temperature is 50-60 ℃. The pressure of the separation kettle II is 5-6 MPa, and the temperature is 30-35 ℃. Most preferably CO in step (3) 2 Supercritical extraction: the pressure of the extraction kettle is 35MPa, and the temperature is 60 ℃; the pressure of the separation kettle I is 11MPa, and the temperature is 55 ℃; the pressure of the separation kettle II is 5MPa, and the temperature is 35 ℃; CO 2 2 The flow rate is 800L/h, and the extraction time is 3 h.
In the step (2) of the invention, when the ratio of the material to the liquid is in the range of 2: 1-1: 2kg/L, particularly the ratio of material to liquid is 1: CO at 1kg/L, low pressure and temperature 2 Under the condition of supercritical extraction, more than 90% of fat-soluble harmful ingredients can be removed, thermosensitive effective ingredients are not damaged, the waste oil content is lower than 2%, and the material loss is extremely low. Further, a small amount of high-concentration ethanol is used as an entrainer to completely remove the residual fat-soluble harmful ingredients, the pressure of a separation kettle II is lower than 8MPa, no solvent is left, and the time for extracting the ganoderma lucidum spore oil is only half of the original time.
The invention adopts twice CO 2 Supercritical extraction is adopted, the efficiency is high, the speed is high, the energy is saved, and fat-soluble harmful ingredients in the ganoderma lucidum spore oil can be completely removed.
Compared with the prior art, the invention has the beneficial effects that: the invention uses ethanol as entrainer, and most fat-soluble harmful components in the raw material ganoderma lucidum spore powder without wall breaking are processed by CO 2 Performing supercritical extraction and elution, and recycling CO from the wall-broken Ganoderma spore powder obtained by wall breaking 2 Supercritical extraction to obtain Ganoderma spore oil without fat-soluble harmful components, with fragrant oil and long storage time. The method has the advantages of quick operation and low energy consumption, is suitable for mass production and processing, effectively removes fat-soluble harmful ingredients, simultaneously retains the effective active ingredients of the ganoderma lucidum spore powder, and gives consideration to the safety, effectiveness and quality controllability of the ganoderma lucidum spore oil.
Detailed Description
The following examples are provided to purchase non-wall-broken Ganoderma spore powder and select representative samples containing fat-soluble harmful components. Wherein, peroxide number: 0.54g/100 g; pesticide residue: 0.03mg/kg of hexachloro cyclohexane, 0.09mg/kg of dichlorodiphenyl trichloroethane, 0.04mg/kg of methyl parathion and 0.12mg/kg of endosulfan; plasticizer: DBP was 4.53mg/kg, DEHP was 5.14 mg/kg; aflatoxin B 1 3.5 mu g/kg, and the total triterpene content is 3.0g/100g, which is taken as the raw material of the non-wall-broken ganoderma lucidum spore powder in the embodiment of the invention.
Example 1
Adding the non-wall-broken Ganoderma spore powder into the non-wall-broken Ganoderma spore powderGranulating with 30% water in a swing granulator, drying in a forced air drying oven at 80 deg.C, controlling water content to be less than 5%, and sieving with 10 mesh sieve to obtain Ganoderma spore powder granule without cell wall breaking. Ethanol with the mass concentration of 95 percent is used as an entrainer (the material-liquid ratio is 1: 1kg/L), and CO is carried out 2 Supercritical extraction, wherein the extraction conditions are as follows: the pressure of the extraction kettle is 20MPa, and the temperature is 50 ℃; the pressure of the separation kettle I is 8MPa, and the temperature is 45 ℃; the pressure of the separation kettle II is 5MPa, and the temperature is 30 ℃; CO 2 2 Extracting at a flow rate of 600L/h for 1.5h to obtain an alcohol-oil mixture and spore powder granules, breaking cell walls of the spore powder granules in a Beili machine to obtain cell wall-broken ganoderma lucidum spore powder, granulating in a disc type feed granule to obtain cell wall-broken ganoderma lucidum spore powder granules, and sieving with a 10-mesh sieve. Ethanol with the mass concentration of 95 percent is used as an entrainer (the material-liquid ratio is 1: 0.1kg/L), and CO is carried out 2 Supercritical extraction, wherein the extraction conditions are as follows: the pressure of the extraction kettle is 35MPa, and the temperature is 60 ℃; the pressure of the separation kettle I is 11MPa, and the temperature is 55 ℃; the pressure of the separation kettle II is 5MPa, and the temperature is 35 ℃; CO 2 2 The flow is 800L/h, the extraction time is 3h, and the degreased particles and the ganoderma lucidum spore oil are obtained.
Through detection, the peroxidation value in the ganoderma lucidum spore oil is 0.02g/100g, pesticide residue is not detected, plasticizer is not detected, and aflatoxin B 1 No detection, no solvent residue. The content of Ganoderma triterpene is 40.5g/100 g.
Example 2
Adding water 30 wt% of the Ganoderma spore powder into the Ganoderma spore powder, granulating in a swing granulator, drying at 80 deg.C in a blast drying oven, controlling water content to be less than 5%, to obtain Ganoderma spore powder granule, and sieving with 10 mesh sieve. Ethanol with the mass concentration of 95 percent is used as an entrainer (the material-liquid ratio range is 1.5: 1kg/L), and CO is carried out 2 Supercritical extraction, wherein the extraction conditions are as follows: the pressure of the extraction kettle is 22MPa, and the temperature is 45 ℃; the pressure of the separation kettle I is 8MPa, and the temperature is 40 ℃; the pressure of the separation kettle II is 5MPa, and the temperature is 35 ℃; CO 2 2 The flow rate is 600L/h, the extraction time is 2h, an alcohol-oil mixture and spore powder particles are obtained, the spore powder particles are subjected to wall breaking in a Beili machine to obtain wall-broken ganoderma lucidum spore powder, the wall-broken ganoderma lucidum spore powder particles are obtained by granulation in a disc type feed granule, and the wall-broken ganoderma lucidum spore powder particles are sieved by a 10-mesh sieve. Is prepared by mass concentrationEthanol with the concentration of 75 percent is used as an entrainer (the material-liquid ratio is 1: 0.15kg/L), and CO is carried out 2 Supercritical extraction, wherein the extraction conditions are as follows: the pressure of the extraction kettle is 40MPa, and the temperature is 65 ℃; the pressure of the separation kettle I is 10MPa, and the temperature is 60 ℃; the pressure of the separation kettle II is 4MPa, and the temperature is 35 ℃; CO 2 2 The flow rate is 700L/h, the extraction time is 4h, and the degreased particles and the ganoderma lucidum spore oil are obtained.
Through detection, the peroxidation value in the ganoderma lucidum spore oil is 0.03g/100g, pesticide residue is not detected, plasticizer is not detected, and aflatoxin B 1 No detection, no solvent residue. The content of Ganoderma triterpene is 40.2g/100 g.
Example 3
Adding water 30 wt% of the Ganoderma spore powder into the Ganoderma spore powder, granulating in a swing granulator, drying at 80 deg.C in a blast drying oven, controlling water content to be less than 5%, to obtain Ganoderma spore powder granule, and sieving with 10 mesh sieve. Ethanol with the mass concentration of 75% is used as an entrainer (the material-liquid ratio is 1: 1.5kg/L), and CO is carried out 2 Supercritical extraction, wherein the extraction conditions are as follows: the pressure of the extraction kettle is 18MPa, and the temperature is 55 ℃; the pressure of the separation kettle I is 7MPa, and the temperature is 50 ℃; the pressure of the separation kettle II is 4MPa, and the temperature is 35 ℃; CO 2 2 The flow is 800L/h, the extraction time is 1h, an alcohol-oil mixture and spore powder particles are obtained, the spore powder particles are subjected to wall breaking in a Beili machine to obtain wall-broken ganoderma lucidum spore powder, the wall-broken ganoderma lucidum spore powder particles are obtained by granulation in a disc type feed granule, and the wall-broken ganoderma lucidum spore powder particles are sieved by a 10-mesh sieve. Ethanol with the mass concentration of 95% is used as an entrainer (the material-liquid ratio is 1: 0.05kg/L), and CO is carried out 2 Supercritical extraction, wherein the extraction conditions are as follows: the pressure of the extraction kettle is 40MPa, and the temperature is 65 ℃; the pressure of the separation kettle I is 12MPa, and the temperature is 50 ℃; the pressure of the separation kettle II is 6MPa, and the temperature is 30 ℃; CO 2 2 The flow rate is 850L/h, the extraction time is 3.5h, and the degreased particles and the ganoderma lucidum spore oil are obtained.
Through detection, the peroxidation value in the ganoderma lucidum spore oil is 0.03g/100g, pesticide residue is not detected, plasticizer is not detected, and aflatoxin B 1 No detection, no solvent residue. The content of Ganoderma triterpene is 39.6g/100 g.
Comparative example 1
Adding water 30 wt% of the non-wall-broken ganoderma spore powder into the non-wall-broken ganoderma spore powder, granulating in a swing granulator, drying at 80 ℃ in an air-blast drying oven, controlling the water content to be lower than 5% to obtain non-wall-broken ganoderma spore powder particles, breaking the wall in a belief machine to obtain wall-broken ganoderma spore powder, granulating in a disc-type feed granule to obtain wall-broken ganoderma spore powder particles, and sieving with a 10-mesh sieve. Subjecting the wall-broken Ganoderma spore powder to CO treatment 2 Supercritical extraction, wherein the extraction conditions are as follows: the pressure of the extraction kettle is 35MPa, and the temperature is 60 ℃; the pressure of the separation kettle I is 11MPa, and the temperature is 55 ℃; the pressure of the separation kettle II is 5MPa, and the temperature is 35 ℃; CO 2 2 The flow is 800L/h, the extraction time is 6h, and the degreased particles and the ganoderma lucidum spore oil are obtained.
Through detection, the peroxide value in the ganoderma lucidum spore oil is 1.33g/100g, and the pesticide residue: 0.13mg/kg of Liuliuliuliu, 0.17mg/kg of DDT, 0.07mg/kg of methyl parathion and 0.20mg/kg of endosulfan; plasticizer: DBP 9.72mg/kg, DEHP 12.59 mg/kg; aflatoxin B 1 10.62. mu.g/kg. The content of Ganoderma triterpene is 35.2g/100 g.
Comparative example 2
Adding water 30 wt% of the non-wall-broken ganoderma spore powder into the non-wall-broken ganoderma spore powder, granulating in a swing granulator, drying at 80 ℃ in an air-blast drying oven, controlling the water content to be lower than 5% to obtain non-wall-broken ganoderma spore powder particles, breaking the wall in a belief machine to obtain wall-broken ganoderma spore powder, granulating in a disc-type feed granule to obtain wall-broken ganoderma spore powder particles, and sieving with a 10-mesh sieve. Ethanol with the mass concentration of 95 percent is used as an entrainer (the material-liquid ratio is 1: 1kg/L), and CO is carried out 2 Supercritical extraction, wherein the extraction conditions are as follows: the pressure of the extraction kettle is 38MPa, and the temperature is 65 ℃; the pressure of the separation kettle I is 12MPa, and the temperature is 60 ℃; the pressure of the separation kettle II is 6MPa, and the temperature is 40 ℃; CO 2 2 The flow rate is 850L/h, the extraction time is 3h, and the degreased particles and the ganoderma lucidum spore oil are obtained.
Through detection, the peroxide value in the ganoderma lucidum spore oil is 0.10g/100g, and the pesticide residue: 0.04mg/kg of methyl parathion and 0.06mg/kg of endosulfan; plasticizer: DBP is 0.22mg/kg, DEHP is 0.98 mg/kg; aflatoxin B 1 0.10 mug/kg; the residual solvent amount was not detected. Ganoderma triterpene contentThe amount was 38.5g/100 g.
Comparative example 3
Adding water 30 wt% of the Ganoderma spore powder into the Ganoderma spore powder, granulating in a swing granulator, oven drying at 80 deg.C in a forced air drying oven, controlling water content to be less than 5%, to obtain Ganoderma spore powder granule, and sieving with 10 mesh sieve. Ethanol with the mass concentration of 95 percent is used as an entrainer (the material-liquid ratio is 1: 1kg/L), and CO is carried out 2 Supercritical extraction, wherein the extraction conditions are as follows: the pressure of the extraction kettle is 20MPa, and the temperature is 50 ℃; the pressure of the separation kettle I is 8MPa, and the temperature is 45 ℃; the pressure of the separation kettle II is 5MPa, and the temperature is 30 ℃; CO 2 2 The flow rate is 600L/h, the extraction time is 1.5h, alcohol-oil mixture and spore powder particles are obtained, the spore powder particles are subjected to wall breaking in a Beili machine to obtain wall-broken ganoderma lucidum spore powder, the wall-broken ganoderma lucidum spore powder particles are obtained by granulation in a disc type feed granule, and the wall-broken ganoderma lucidum spore powder particles are sieved by a 10-mesh sieve. Carrying out CO 2 Supercritical extraction, wherein the extraction conditions are as follows: the pressure of the extraction kettle is 35MPa, and the temperature is 60 ℃; the pressure of the separation kettle I is 11MPa, and the temperature is 55 ℃; the pressure of the separation kettle II is 5MPa, and the temperature is 35 ℃; CO 2 2 The flow is 800L/h, the extraction time is 3h, and the degreased particles and the ganoderma lucidum spore oil are obtained.
Through detection, the peroxide value in the ganoderma lucidum spore oil is 0.08g/100g, and the pesticide residue: 0.02mg/kg of methyl parathion and 0.05mg/kg of endosulfan; plasticizer: DBP is 0.31mg/kg, DEHP is 1.25 mg/kg; aflatoxin B 1 0.10. mu.g/kg, and no solvent residue was detected. The content of Ganoderma triterpene is 39.3g/100 g.
Comparative example 4
Adding water 30 wt% of the Ganoderma spore powder into the Ganoderma spore powder, granulating in a swing granulator, drying at 80 deg.C in a forced air drying oven, controlling water content to be less than 5%, and sieving with 10 mesh sieve to obtain Ganoderma spore powder granule. Ethanol with the mass concentration of 95% is used as an entrainer, and the material-liquid ratio range is 1: 1kg/L of CO, CO 2 Supercritical extraction, wherein the extraction conditions are as follows: the pressure of the extraction kettle is 20MPa, and the temperature is 50 ℃; the pressure of the separation kettle I is 8MPa, and the temperature is 45 ℃; the pressure of the separation kettle II is 5MPa, and the temperature is 30 ℃; CO 2 2 The flow rate is 600L/h, the extraction time is 1.5h, and an alcohol-oil mixture and spore powder particles are obtainedBreaking cell wall of spore powder granules in a Beili machine to obtain cell wall-broken Ganoderma spore powder, granulating in disc feed granules to obtain cell wall-broken Ganoderma spore powder granules, and sieving with 10 mesh sieve.
Ethanol with the mass concentration of 95 percent is used as an entrainer (the material-liquid ratio is 1: 0.1kg/L), and CO is carried out 2 Supercritical extraction, wherein the extraction conditions are as follows: the pressure of the extraction kettle is 35MPa, and the temperature is 60 ℃; the pressure of the separation kettle I is 8MPa, and the temperature is 55 ℃; the pressure of the separation kettle II is 5MPa, and the temperature is 35 ℃; CO 2 2 The flow rate is 800L/h, the extraction time is 3h, and the degreased particles and the ganoderma lucidum spore oil are obtained.
Through detection, the peroxidation value in the ganoderma lucidum spore oil is 0.02g/100g, pesticide residue is not detected, plasticizer is not detected, and aflatoxin B 1 Not detected, the residual amount of solvent was 25 mg/kg. The content of Ganoderma triterpene is 38.8g/100 g.
1. The method for measuring the content of ganoderma triterpenoids in the ganoderma lucidum spore oil product prepared by the embodiment of the invention comprises the following steps:
(1) preparation of control solutions
Precisely weighing 10mg of oleanolic acid control sample dried at 105 deg.C to constant weight, placing in a 50ml volumetric flask, adding chloroform to dissolve and diluting to scale to obtain oleanolic acid control sample solution.
(2) Preparation of the Standard Curve
Precisely sucking standard oleanolic acid reference substance solution 0.1, 0.2, 0.4, 0.6, 0.8ml, respectively placing into 10ml colorimetric tube, heating to volatilize solvent, adding vanillin solution 0.5ml of 80g/L and sulphuric acid solution (taking water 25ml, adding sulphuric acid to dissolve to 100ml)5.0ml, mixing, keeping temperature in water bath at 60 deg.C for 30min, taking out, and placing in cold water bath for 15 min. In a 1cm cuvette, the reagent blank solution is used as a reference for zero adjustment, the absorbance is measured at the wavelength of 500nm, and the absorbance is used for regression of the concentration to draw a standard curve.
(3) Preparation of test solution
Weighing 120-150 mg of ganoderma spore oil sample, adding trichloromethane, and dissolving in a 100ml volumetric flask to obtain a test solution.
(4) Assay method
Precisely sucking 0.2ml to 10ml of sample solution into a colorimetric tube, operating the method according to the preparation item of a standard curve from the step of heating to volatilize the solvent, measuring the absorbance, reading the oleanolic acid content in the sample solution from the standard curve, and calculating to obtain the oleanolic acid.
(5) Formula for calculation
In the formula:
w represents the content of ganoderma triterpene in the sample, g/100 g;
c- - -oleanolic acid content, mg/ml, found from the standard curve;
v is the volume of the colorimetric solution, ml;
f- - -dilution factor;
m-mass of sample, mg.
(6) As a result, the
And calculating the content of the ganoderma triterpene in the sample according to the standard curve, and calculating by combining the mass of the sample.
The detection of the content of the total triterpenoids refers to a method specified in the determination of the total triterpenoids in the health-care food, namely twenty in 2020 edition according to the guiding principle of health-care food physicochemical and health index detection and evaluation technology.
2. The fat-soluble harmful component regulation limit requirement and the detection method are as follows:
the peroxide value (calculated by ganoderma spore oil) is regulated to be less than or equal to 0.20g/100g in the catalog health food raw material ganoderma lucidum spore powder. The detection method comprises the following steps: first-law titration method for determining peroxide value in GB 5009.227-2016 food safety national standard food
The requirement that 33 forbidden pesticides of medicinal materials and decoction pieces (plants) cannot be detected (the limit of quantification cannot be exceeded) is newly added in the general rules of 0212 verification of medicinal materials and decoction pieces in the universal rules of the four ministry of the 2020 version of the pharmacopoeia of the people's republic of China: less than or equal to 0.1mg/kg of hexachloro cyclohexane, less than or equal to 0.1mg/kg of dichlorodiphenyl trichloroethane, less than or equal to 0.02mg/kg of methyl parathion and less than or equal to 0.05mg/kg of endosulfan. The detection method comprises the following steps: method for measuring pesticide residue in the fifth method of medicinal materials and decoction pieces (plants) of the fifth method of measuring pesticide residue in the fourth 2341 part of the 2020 pharmacopoeia of the people's republic of China
The letter "office of Ministry of health" for reporting the maximum residual amounts of phthalic acid ester substances in foods and food additives (official supervision letter No. 2011 551) stipulates that the maximum residual amounts of DEHP and DBP in foods and food additives are 1.5 and 0.3mg/kg, respectively. The detection method comprises the following steps: second-method gas chromatography-mass spectrometry external standard method for determining phthalate in GB 5009.271-2016 food safety national standard food
GB 2761-containing 2017 food safety national standard food contains mycotoxin limit regulation, and plant oil contains aflatoxin B 1 The limit amount is 10 mug/kg. The detection method comprises the following steps: determination of aflatoxin B family and aflatoxin G family in GB 5009.22-2016 food safety national standard food by second method high performance liquid chromatography-pre-column derivatization method
The residual quantity of the solvent specified in the GB 2716-2018 food safety national standard vegetable oil is less than or equal to 20 mg/kg. The detection method comprises the following steps: and (3) measuring the residual quantity of the solvent in GB 5009.262-2016 food safety national standard food.
Claims (9)
1. A method for removing fat-soluble harmful ingredients in ganoderma lucidum spore oil is characterized by comprising the following steps:
(1) adding 30-35% of water into the ganoderma lucidum spore powder without wall breaking, granulating, drying at 70-80 ℃ until the water content is lower than 5%, and sieving with a 10-20-mesh sieve to obtain ganoderma lucidum spore powder particles without wall breaking;
(2) ethanol with the mass concentration of 75-95% is used as an entrainer, and the material-liquid ratio is 2: 1-1: 2kg/L of a catalyst, CO 2 Supercritical extraction, wherein the extraction conditions are as follows: the pressure of the extraction kettle is 15-22 MPa, and the temperature is 45-60 ℃; the pressure of the separation kettle I is 6-10 MPa, and the temperature is 35-55 ℃; the pressure of the separation kettle II is 4-6 MPa, and the temperature is 20-40 ℃; CO 2 2 The flow rate is 400-800L/h, the extraction time is 1-2 h, an alcohol-oil mixture and spore powder particles are obtained, the spore powder particles are subjected to wall breaking to obtain wall-broken ganoderma lucidum spore powder, granulation is carried out to obtain wall-broken ganoderma lucidum spore powder particles, and the wall-broken ganoderma lucidum spore powder particles are sieved by a 10-mesh sieve;
(3) ethanol with the mass concentration of 75-95% is used as an entrainer, and the material-liquid ratio range is 1: 0.05-1: 0.15kg/L, CO 2 Supercritical extraction, wherein the extraction conditions are as follows: the pressure of the extraction kettle is 30-40 MPa, and the temperature is 50-70 ℃; the pressure of the separation kettle I is 10-12 MPa, and the temperature is 50-60 ℃; the pressure of the separation kettle II is 4-6 MPa, and the temperature is 30-40 ℃; CO 2 2 The flow rate is 700-900L/h, and the extraction time is 2.5-4.5 h, so that the defatted particles and the ganoderma lucidum spore oil are obtained.
2. The method for removing fat-soluble harmful ingredients from ganoderma lucidum spore oil according to claim 1, wherein the material-to-liquid ratio in the step (2) is 1-1.5: 1 to 1.5 kg/L.
3. The method for removing fat-soluble harmful ingredients from ganoderma lucidum spore oil according to claim 1, wherein the CO in the step (2) 2 The supercritical extraction adopts an extraction kettle with the pressure of 18-22 MPa and the temperature of 45-60 ℃.
4. The method for removing fat-soluble harmful ingredients from ganoderma lucidum spore oil as claimed in claim 3, wherein the pressure of the separation kettle I in the step (2) is 7-8 MPa, and the temperature is 40-50 ℃.
5. The method for removing fat-soluble harmful ingredients from ganoderma lucidum spore oil as claimed in claim 4, wherein the pressure of the separation kettle II in the step (2) is 4-5 MPa, and the temperature is 30-35 ℃.
6. The method for removing fat-soluble harmful ingredients from ganoderma lucidum spore oil as claimed in claim 1, wherein: the material-liquid ratio range in the step (3) is 1: 0.1 kg/L.
7. The method for removing fat-soluble harmful ingredients from ganoderma lucidum spore oil as claimed in claim 1, wherein: CO in the step (3) 2 Supercritical extraction: the pressure of the extraction kettle is 35-40 MPa, and the temperature is 60-65 ℃.
8. The method for removing fat-soluble harmful ingredients from ganoderma lucidum spore oil as claimed in claim 1, wherein: in the step (3), the pressure of the separation kettle I is 10-12 MPa, and the temperature is 50-60 ℃.
9. The method for removing fat-soluble harmful ingredients from ganoderma lucidum spore oil as claimed in claim 1, wherein: the pressure of the separation kettle II is 5-6 MPa, and the temperature is 30-35 ℃.
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| WO2023241456A1 (en) * | 2022-06-15 | 2023-12-21 | 南京中科药业有限公司 | Method for removing fat-soluble harmful ingredients in ganoderma lucidum spore oil |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4055674A (en) * | 1975-06-17 | 1977-10-25 | Asahi Kasei Kogyo Kabushiki Kaisha | Method for the removal of aflatoxin from cereals, oil seeds and feedstuffs |
| CN102041163A (en) * | 2011-01-05 | 2011-05-04 | 南昌同心紫巢生物工程有限公司 | Multi-body multi-stage supercritical CO2 extraction method of ganoderma lucidum spore oil |
| CN102965192A (en) * | 2012-11-05 | 2013-03-13 | 广州宝兴生物科技有限公司 | Method for removing plasticizer residual and contaminant from ganoderma lucidum spore oil raw materials |
| CN102961416A (en) * | 2012-11-05 | 2013-03-13 | 广州宝兴生物科技有限公司 | Method for removing plasticizer residual and contaminant from ganoderma lucidum spore powder raw materials |
| CN104073344A (en) * | 2014-07-16 | 2014-10-01 | 江苏斯威森生物医药工程研究中心有限公司 | Extracting method for ganoderma lucidum spore oil |
| CN106398861A (en) * | 2016-10-31 | 2017-02-15 | 中山大学 | Entrainer-containing supercritical CO2 extraction method of ganderma lucidum spore oil |
| US20170360802A1 (en) * | 2015-08-20 | 2017-12-21 | Guangzhou Polysarm Bioscience Corp. | Enrichment Method of Ergosterol Peroxide from Sporoderm-Broken Ganoderma Lucidum Spore Powder |
| CN112587554A (en) * | 2020-12-15 | 2021-04-02 | 福建仙芝楼生物科技有限公司 | Ganoderma spore oil with gastric mucosa protecting effect, and its preparation method and equipment |
| US20210269615A1 (en) * | 2018-11-16 | 2021-09-02 | Zhejiang University | Method for Removing Volatile Organic Compounds from Sponge by Using Supercritical or Subcritical Fluid |
| WO2022105726A1 (en) * | 2020-11-18 | 2022-05-27 | 中科健康产业集团股份有限公司 | Production method for lycopene-containing granules with efficient antioxidation effect |
Family Cites Families (1)
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|---|---|---|---|---|
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-
2023
- 2023-06-08 WO PCT/CN2023/099177 patent/WO2023241456A1/en unknown
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4055674A (en) * | 1975-06-17 | 1977-10-25 | Asahi Kasei Kogyo Kabushiki Kaisha | Method for the removal of aflatoxin from cereals, oil seeds and feedstuffs |
| CN102041163A (en) * | 2011-01-05 | 2011-05-04 | 南昌同心紫巢生物工程有限公司 | Multi-body multi-stage supercritical CO2 extraction method of ganoderma lucidum spore oil |
| CN102965192A (en) * | 2012-11-05 | 2013-03-13 | 广州宝兴生物科技有限公司 | Method for removing plasticizer residual and contaminant from ganoderma lucidum spore oil raw materials |
| CN102961416A (en) * | 2012-11-05 | 2013-03-13 | 广州宝兴生物科技有限公司 | Method for removing plasticizer residual and contaminant from ganoderma lucidum spore powder raw materials |
| CN104073344A (en) * | 2014-07-16 | 2014-10-01 | 江苏斯威森生物医药工程研究中心有限公司 | Extracting method for ganoderma lucidum spore oil |
| US20170360802A1 (en) * | 2015-08-20 | 2017-12-21 | Guangzhou Polysarm Bioscience Corp. | Enrichment Method of Ergosterol Peroxide from Sporoderm-Broken Ganoderma Lucidum Spore Powder |
| CN106398861A (en) * | 2016-10-31 | 2017-02-15 | 中山大学 | Entrainer-containing supercritical CO2 extraction method of ganderma lucidum spore oil |
| US20210269615A1 (en) * | 2018-11-16 | 2021-09-02 | Zhejiang University | Method for Removing Volatile Organic Compounds from Sponge by Using Supercritical or Subcritical Fluid |
| WO2022105726A1 (en) * | 2020-11-18 | 2022-05-27 | 中科健康产业集团股份有限公司 | Production method for lycopene-containing granules with efficient antioxidation effect |
| CN112587554A (en) * | 2020-12-15 | 2021-04-02 | 福建仙芝楼生物科技有限公司 | Ganoderma spore oil with gastric mucosa protecting effect, and its preparation method and equipment |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023241456A1 (en) * | 2022-06-15 | 2023-12-21 | 南京中科药业有限公司 | Method for removing fat-soluble harmful ingredients in ganoderma lucidum spore oil |
| CN117065453A (en) * | 2023-08-17 | 2023-11-17 | 广东青云山药业有限公司 | Device and process for removing phthalate plasticizers in ganoderma lucidum triterpene extract |
| CN117065453B (en) * | 2023-08-17 | 2024-06-07 | 广东青云山药业有限公司 | Device and process for removing phthalate plasticizers in ganoderma lucidum triterpene extract |
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| CN115125059B (en) | 2024-03-26 |
| WO2023241456A1 (en) | 2023-12-21 |
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