Supercritical CO2 extraction of Ganoderma lucidum Spores oil
Supercritical co2 extraction process
Pulverization degree:80 mesh
Extraction pressure: 25 MPa
Extraction temperature: 45°C
Separation kettle Ⅰ pressure: 0.5 MPa
Extraction time: 180 min
Ganoderma spore oil is a lipid extract of Ganoderma lucidum spores, which accounts for 20% to 35% of the total weight of the spores, and is rich in biologically active ingredients, such as triterpenoid ganoderic acid, unsaturated fatty acids and steroids. Ganoderma spore oil has special physiological effects, and has broad market prospects in the field of health products and medicine.
The supercritical extraction device is used to extract the lucid ganoderma spore powder after breaking the wall.
Mainly study the influence of single factors such as extraction pressure, extraction temperature and extraction time on the extraction rate of Ganoderma lucidum spore oil during supercritical CO2 extraction.
The test results show that the optimal extraction conditions are extraction pressure 25 MPa, extraction temperature 45 ℃, and extraction time 3 h. Under this optimal extraction process condition, the highest extraction rate is 28.8%. The Ganoderma lucidum spore oil is golden and translucent, and the quality is good.
Ganoderma lucidum and ganoderma spore powder
Ganoderma lucidum, also known as fungus Ganoderma lucidum, or Ganoderma lucidum, is a genus of Ganoderma lucidum in the family Basidiomycetes Polyporus. It is a mushroom parasitic on the roots of oak and other broad-leaved trees. Umbrella-shaped, hard, woody, kidney-capped or semicircular, purple-brown with paint-like luster. The ancient Orientals praised Ganoderma lucidum as a "magic panacea" that can be brought back to life, and a "celestial herb" that cures all diseases. Modern scientific and clinical medical studies have proved that Ganoderma lucidum contains rich nutrients and biologically active substances, and it has a tonic and strong effect. The effect is the most ideal natural medicine and health food for human beings.
The Ganoderma lucidum spore powder is the seed of Ganoderma lucidum. It is the extremely tiny egg-shaped reproductive cells ejected from Ganoderma lucidum pleats during the growth and maturity of Ganoderma lucidum. It is only 4-6 micrometers and is a living organism. The spore powder contains all the active essences of Ganoderma lucidum. It contains 18 kinds of active amino acids, more than 20 kinds of polysaccharides, alkaloids, organic germanium, terpenoids, various vitamins and trace elements and other pharmacologically active ingredients. Longevity and longevity can significantly improve the body's immune function and promote the production of IgM and IgG. It has antiviral, anticancer, tumor suppressing, hypoglycemic and other functions. Its medicinal value is much higher than that of Ganoderma lucidum fruiting body and mycelium.
Principles and advantages of supercritical CO2 fluid extraction
The principle of supercritical CO2 fluid extraction (SFE) is to use the relationship between the solubility and density of supercritical fluids, that is, to use the influence of pressure and temperature factors on the solubility of supercritical fluids. Under supercritical conditions, the supercritical fluid is brought into contact with the material to be separated so that it can selectively extract components with different polarities, boiling points, and molecular weights in sequence. At the same time, the extracts corresponding to each pressure range are not single, but the conditions can be controlled to obtain the optimal ratio of the mixture, and then by means of depressurization and temperature increase, the The supercritical fluid can be changed into ordinary gas, and the extracted material can be completely or basically precipitated to achieve the effect of separation and purification. Therefore, the supercritical CO2 fluid extraction process is a combination of extraction and separation processes.
The supercritical fluid can effectively separate and purify the extract, and can also avoid the process of heating and recovery of the solvent generated when extracting with a general organic solvent, so there is no series of problems such as residual organic solvent, and it is relatively relative to the temperature. Sensitive medicines and foods, especially for more volatile products, are more conducive to better preservation and can guarantee higher quality of products. Therefore, supercritical carbon dioxide extraction technology has become a more expensive pure natural product. Its preferred process.
Compared with the traditional chemical extraction method, carbon dioxide supercritical extraction has the following outstanding advantages:
(1) Substances can be extracted relatively close to room temperature and under the conditions of carbon dioxide gas, which can effectively suppress the oxidation and escape of heat-sensitive substances. Therefore, in the extract, all the components of the extracted plant can be maintained, and the high boiling point, low volatility, and easily pyrolyzed substances can be selected for extraction below their boiling point temperature conditions;
(2) Supercritical CO2 fluid extraction is one of the purest substance extraction methods at present, and the entire process does not require organic solvents, so there is no residual organic solvent in the obtained extract, and can effectively prevent the extraction process The organic solvents in Shanghai cause pollution to the human body and the environment;
(3) SFE can combine the extraction process and the separation process into one. When the CO2 fluid saturated with dissolved matter flows through the separator, due to the decrease in pressure, the gas and liquid separation of the CO2 and the extract are rapidly generated, and Immediate separation, which not only has a high extraction efficiency, but also can obtain a higher purity extract;
(4) Carbon dioxide is an inert gas, therefore, no chemical reaction will occur during the entire extraction process, and CO2 is a non-flammable gas, tasteless, odorless, non-toxic, and has good safety performance;
(5) Carbon dioxide has high purity, is easy to obtain, and is recycled in the production process, which is beneficial to environmental protection;
(6) Both pressure and temperature can be parameters that regulate the extraction process, and the purpose of extraction can be achieved by changing the temperature and pressure. Under the condition of fixed pressure, changing the temperature condition can separate the material; while the temperature condition is fixed, changing the pressure condition can also cause the extract to be separated, so it has a faster extraction speed. However, this technology also has some shortcomings, high production cost and high equipment requirements, so it is currently only suitable for the extraction of active substances and oils with small output and high added value, such as bitter substances in olives and grape seed oil, evening primrose oil, Gardenia fruit oil and other active ingredients of traditional Chinese medicine and small varieties of oil.
Supercritical CO2 extraction technology is used to produce Ganoderma spore oil. While ensuring product safety and extraction rate, it maximizes the content of active ingredients and maintains the unique Ganoderma lucidum aroma.
Effect of extraction pressure on extraction rate:
According to the reference, 100 g of broken lucid ganoderma spore powder was placed in a 1 L extraction kettle at an extraction temperature of 40° C. extraction time 3 h and a separation pressure of 6 MPa was selected at 10 MPa, 15 MPa, 20 MPa, 25 MPa, 30 MPa, 35 A total of 6 different gradients of MPa were used for extraction pressure test to get the best extraction pressure.
Weigh 100 g of broken wall Ganoderma lucidum spore powder and place it in a 1 L extraction kettle at a separation pressure of 6 MPa for an extraction time of 3 h and the optimal extraction pressure conditions of 20°C, 25°C, 30°C, 35°C and 40°C. There are 7 different gradients at 45°C and 50°C to perform the extraction temperature test to obtain the optimal extraction temperature T.
Weigh 100 g of broken wall Ganoderma lucidum spore powder and place it in a 1 L extraction kettle at a separation pressure of 6 MPa℃ and optimal extraction pressure and extraction temperature for 30 min, 60 min, 90 min, 120 min, 150 min, Eight different gradients of 180 min, 210 min and 240 min were used for extraction time test to get the best extraction time t.
Effect of extraction pressure on the extraction rate of Ganoderma lucidum spore oil:
Under the conditions of extraction temperature 40 ℃ extraction time 3 h and separation pressure 6 MPa, the effect of extraction pressure on the yield of Ganoderma lucidum spore oil was studied
Before the extraction pressure reached 25 MPa, the extraction rate of Ganoderma spore oil increased rapidly with the increase of pressure. But as the pressure continues to increase, the oil extraction rate tends to be in equilibrium. The extraction pressure can increase the solubility of the solute by increasing the concentration of CO2, thereby affecting the extraction effect, but the increase of the extraction pressure will also reduce the diffusion coefficient of the solute in the solvent, hindering the extraction process. In addition, the excessively high extraction pressure requires high pressure resistance of the equipment and increases unsafe factors. Therefore, the extraction pressure was chosen to be 25 MPa.
Effect of extraction temperature on extraction rate of Ganoderma lucidum spore oilUnder the extraction pressure of 6 MPa and the extraction time of 3 h and the optimal extraction pressure, the effect of extraction temperature on the yield of Ganoderma lucidum spore oil was investigated.
When the extraction temperature is low, the extraction rate of Ganoderma lucidum spore oil increases rapidly with the increase of temperature. The oil extraction rate reached its highest value at a temperature of 45°C. After that, as the extraction temperature further increased, the oil extraction rate showed a downward trend. This is because supercritical CO2 has a double effect on the solubility of the extracted material: on the one hand, the extraction temperature can increase the diffusion coefficient of the solute in CO2, thereby improving the extraction rate; on the other hand, the density of supercritical CO2 may vary with the temperature Increase and decrease, so that the solubility of solute in CO2 is reduced, hindering further extraction. Therefore, considering the comprehensive consideration, the optimal extraction temperature is 45℃.
Effect of extraction time on the extraction rate of Ganoderma lucidum spore oilUnder the conditions of extraction pressure of 25 MPa and extraction temperature of 45℃, the effect of extraction time on the extraction rate of Ganoderma lucidum spore oil was studied. At the beginning of extraction, the yield of Ganoderma spore oil increased significantly with the increase of time. But when the extraction time exceeds 3 h, the oil yield reaches equilibrium and there is no longer a large fluctuation. This is because in the early stage of extraction, the solute and the solvent have not been fully contacted. With the extension of time, a good mass transfer effect is achieved. In the later stage of extraction, as the content of the substance to be extracted in the sample decreases, the oil extraction rate no longer changes. Prolonging the extraction time will only waste energy consumption and CO2 consumption. From economic considerations, the extraction time is selected for 3 h.
Supercritical CO2 extraction technology is an emerging extraction, separation and purification technology in food, medicine, health care products and other industries. Compared with the traditional chemical solvent extraction method, it has the following characteristics: no chemical solvent consumption and residue, no pollution, and avoids extracts Thermal cracking at high temperature to protect the activity of physiological substances: simple process, low energy consumption, non-toxic extractant, and easy recovery. Ganoderma lucidum spore oil is extracted by supercritical CO2 extraction method, which can effectively extract the ganoderma spore oil, and the extract has high purity and positive fragrance.
In this experiment, the optimal process conditions for supercritical CO2 extraction of Ganoderma lucidum spore oil are extraction pressure 25 MPa, extraction temperature 45 ℃, extraction time 3 h. Under this condition, the extracted Ganoderma spore oil becomes golden and translucent, and the highest extraction rate is 28.8%.