Ganoderma lucidum spore oil efficient extraction device and extraction process

Abstract

The invention relates to the technical field of ganoderma lucidum spore oil extraction, and discloses an efficient ganoderma lucidum spore oil extraction device and process, the process comprises pretreatment, supercritical extraction, separation and purification and post-treatment.The pretreatment device comprising a microwave wall breaking unit is additionally arranged, efficient cell wall breaking treatment is carried out on ganoderma lucidum spore raw materials, and the extraction efficiency is improved; the compact structure of a spore wall is destroyed, so that internal grease is easier to release, and the extraction efficiency of a subsequent extraction process and the yield of a target product are improved; by adopting an extraction system which takes supercritical carbon dioxide as a main body and cooperates with an entrainer, the specific high diffusivity and strong dissolving capacity of supercritical fluid are utilized, and the solubilizing effect of the entrainer on polar components is combined, so that fat-soluble and partial polar active components in the ganoderma lucidum spores are efficiently and selectively extracted; the extraction rate and the comprehensive quality of an extraction product are improved.

Description

Technical Field

[0001] This invention relates to the field of Ganoderma lucidum spore oil extraction technology, specifically to a high-efficiency Ganoderma lucidum spore oil extraction device and extraction process. Background Technology

[0002] Ganoderma lucidum spore oil is an oily substance extracted from Ganoderma lucidum spore powder. It is often made into transparent capsules. Its quality can be distinguished by color and smell. Those with a clear color and fragrant smell have higher purity. The main active ingredient is Ganoderma lucidum triterpenes, which have the effects of inhibiting tumors and regulating immunity. Because it is easily oxidized and degraded, domestic research institutions have improved its stability by adding the natural antioxidant vitamin E.

[0003] Currently, due to the dense spore wall structure and the easy oxidation and degradation of active ingredients during the extraction of Ganoderma lucidum spore oil, traditional extraction processes using mechanical wall breaking and organic solvent extraction methods cannot effectively destroy the spore wall structure and easily lead to solvent residue and loss of heat-sensitive components. This may result in low extraction efficiency and insufficient product purity, making it impossible to guarantee the high quality and high yield of Ganoderma lucidum spore oil.

[0004] Therefore, a high-efficiency extraction device and extraction process for Ganoderma lucidum spore oil are proposed to solve the above problems. Summary of the Invention

[0005] To address the shortcomings of existing technologies, this invention provides a high-efficiency extraction device and extraction process for Ganoderma lucidum spore oil, which solves the problems mentioned in the background technology, such as the inability to effectively destroy the spore wall structure, the easy occurrence of solvent residue and loss of heat-sensitive components, which may result in low extraction efficiency and insufficient product purity, and the inability to guarantee the high quality and high yield of Ganoderma lucidum spore oil.

[0006] To achieve the above objectives, the present invention provides the following technical solution: a high-efficiency extraction process for Ganoderma lucidum spore oil, comprising the following steps: Step 1: Pre-treatment. Select Ganoderma lucidum spore raw materials, screen them to remove impurities, and then use microwave-assisted cell wall breaking to break the spore walls. Step 2: Supercritical extraction. Place the broken Ganoderma lucidum spores in a supercritical extraction device, use carbon dioxide as the extraction solvent, control the extraction pressure at 20-40 MPa, the extraction temperature at 40-60℃, the carbon dioxide flow rate at 10-30 kg / h, and the extraction time at 1-3 hours, so that the Ganoderma lucidum spore oil dissolves in the supercritical fluid. Step 3: Separation and purification. The extracted supercritical fluid is introduced into a separator. By reducing the pressure to 5-10 MPa and the temperature to 20-30℃, carbon dioxide is vaporized and separated to obtain crude Ganoderma lucidum spore oil. The crude oil is then purified, including deacidification and heavy metal removal. Deacidification is performed by adjusting the acid value to 0.5-1.0 mg / g using an alkali refining method, and heavy metal removal is performed by chelating agent treatment. Step 4: Post-processing. The purified Ganoderma lucidum spore oil is crystallized at low temperature to remove impurities. Then, it is filtered to obtain refined Ganoderma lucidum spore oil. The peroxide value is controlled to be below 0.25g / 100g. The total triterpenoid content in the final product, calculated as oleanolic acid, is not less than 28%, and the moisture and volatile matter content is not higher than 0.1%.

[0007] Preferably, the cell wall breaking process in step one adopts microwave-assisted cell wall breaking method, with microwave power set to 300-500W, processing time of 5-10 minutes, cell wall breaking rate of not less than 95%, and spore particle size controlled within the range of 50-100 micrometers after cell wall breaking.

[0008] Preferably, in the supercritical extraction process of step two, the flow rate of carbon dioxide is controlled by a mass flow meter, and an entrainer is added. The entrainer is ethanol or water, and the amount added is 5-10% of the mass of carbon dioxide.

[0009] Preferably, the purification process in step three further includes a microbial control step, which employs microfiltration membrane filtration.

[0010] Preferably, the crystallization process in step four is carried out at -5 to 5°C for 2 to 4 hours, and a centrifuge is used to separate the crystallized impurities. The relative density of the product is controlled within the range of 0.910 to 0.920, and the contents of aflatoxin B1 and benzo[a]pyrene are less than 10 μg / kg and 0.5 μg / kg, respectively.

[0011] Preferably, the process further includes a resource recovery step, in which the carbon dioxide gas generated by the separation unit is condensed and liquefied and then returned to the carbon dioxide supply system for recycling, with a recovery rate of not less than 95%. Meanwhile, the extraction residue is dried and pulverized for reuse as feed additives or organic fertilizers.

[0012] A high-efficiency extraction device for Ganoderma lucidum spore oil includes: The extraction unit consists of an extraction vessel, a carbon dioxide supply system, a pressure regulator, and a temperature controller. The extraction vessel is used to contain Ganoderma lucidum spore raw materials. The carbon dioxide supply system injects carbon dioxide into the extraction vessel through a high-pressure pump. The pressure regulator controls the extraction pressure within the range of 20-40 MPa. The temperature controller maintains the extraction temperature within the range of 40-60℃. The separation unit, connected to the extraction unit via pipelines, includes a primary separator and a secondary separator. The primary separator reduces the pressure to 10-15 MPa to separate some carbon dioxide, and the secondary separator further reduces the pressure to 5-10 MPa and cools the temperature to 20-30°C to achieve complete extraction of Ganoderma lucidum spore oil. The purification unit includes a deacidification tank and a heavy metal removal device. The deacidification tank has a built-in stirrer and pH sensor for alkali refining treatment, and the heavy metal removal device uses a chelating resin bed. The control system is integrated with a PLC programmable logic controller to monitor extraction pressure, temperature, flow rate and purification parameters in real time, and to set and adjust process conditions through a human-machine interface.

[0013] Preferably, the extraction vessel of the extraction unit adopts a double-jacket design, with circulating heat transfer oil flowing through the jacket. The temperature controller adjusts the temperature through a PID algorithm, with a fluctuation range not exceeding ±1℃. The extraction vessel is equipped with a stirring paddle with a stirring speed of 50-100 r / min. The output formula of the PID control algorithm is as follows: ; ; in This indicates the output signal of the controller. Indicates the error signal. This is the extraction temperature setting. It is a real-time monitored temperature value. Represents the proportional gain coefficient. Represents the integral gain coefficient. Represents the differential gain coefficient. Represents a time variable. It is an integral variable.

[0014] Preferably, both the primary and secondary separators of the separation unit are equipped with pressure sensors and automatic pressure relief valves. The pressure relief valves have a response time of less than 1 second, and the inner walls of the separators are coated with polytetrafluoroethylene to prevent Ganoderma lucidum spore oil from adhering.

[0015] Preferably, the PLC programmable logic controller of the control system integrates a data acquisition module to record extraction pressure, temperature, flow rate and purification parameters in real time, and transmits the data to the cloud server via wireless transmission to realize remote monitoring and fault diagnosis. At the same time, the device is equipped with a safety interlock system to automatically shut down in case of overpressure or overtemperature.

[0016] Compared with the prior art, the present invention provides a high-efficiency extraction device and extraction process for Ganoderma lucidum spore oil, which has the following beneficial effects: 1. In this invention, by adding a pretreatment device containing a microwave cell wall breaking unit, the Ganoderma lucidum spore raw material is subjected to efficient cell wall breaking treatment, which destroys the dense structure of the spore wall and makes the internal oil easier to release, thereby improving the extraction efficiency of the subsequent extraction process and the yield of the target product.

[0017] 2. In this invention, by employing an extraction system based on supercritical carbon dioxide and synergistically using an entrainer, the high diffusivity and strong solubility of supercritical fluids are utilized, combined with the solubilizing effect of the entrainer on polar components, to achieve efficient and selective extraction of lipid-soluble and some polar active components from Ganoderma lucidum spores, thereby improving the extraction rate and the overall quality of the extraction product.

[0018] 3. In this invention, by integrating a purification device that includes deacidification and heavy metal removal units, the crude oil obtained from extraction is subjected to multi-stage series purification treatment to remove free fatty acids and potential heavy metal impurities, optimize the color, acid value and hygiene and safety indicators of the spore oil, and finally obtain a high-purity, high-quality Ganoderma lucidum spore oil product. Detailed Implementation

[0019] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0020] Example 1: A high-efficiency extraction process for Ganoderma lucidum spore oil, comprising the following steps: Step 1: Pre-treatment. Select Ganoderma lucidum spore raw materials, screen them to remove impurities, and then use microwave-assisted cell wall breaking to break the spore walls. Step 2: Supercritical extraction. Place the broken Ganoderma lucidum spores in a supercritical extraction device, use carbon dioxide as the extraction solvent, control the extraction pressure at 20 MPa, the extraction temperature at 40℃, the carbon dioxide flow rate at 10 kg / h, and the extraction time at 1 hour, so that the Ganoderma lucidum spore oil dissolves in the supercritical fluid. Step 3: Separation and purification. The extracted supercritical fluid is introduced into a separator. By reducing the pressure to 5 MPa and the temperature to 20°C, carbon dioxide is vaporized and separated to obtain crude Ganoderma lucidum spore oil. The crude oil is then purified, including deacidification and heavy metal removal. Deacidification is performed by adjusting the acid value to 0.5 mg / g using an alkali refining method, and heavy metal removal is performed by chelating agent treatment. Step 4: Post-processing. The purified Ganoderma lucidum spore oil is crystallized at low temperature to remove impurities. Then, it is filtered to obtain refined Ganoderma lucidum spore oil. The peroxide value is controlled to be below 0.25g / 100g. The total triterpenoid content in the final product, calculated as oleanolic acid, is not less than 28%, and the moisture and volatile matter content is not higher than 0.1%.

[0021] In step one, the cell wall breaking process adopts microwave-assisted cell wall breaking method, with microwave power set at 300W, processing time of 5 minutes, cell wall breaking rate of not less than 95%, and spore particle size controlled at 50 micrometers after cell wall breaking.

[0022] In step two, during the supercritical extraction process, the flow rate of carbon dioxide is controlled by a mass flow meter, and an entrainer is added. The entrainer is ethanol or water, and the amount added is 5% of the mass of carbon dioxide.

[0023] Step three of the purification process also includes a microbial control step, which involves filtration using a microfiltration membrane.

[0024] In step four, the crystallization process was carried out at -5°C for 2 hours. A centrifuge was used to separate the crystallized impurities. The relative density of the product was controlled at 0.910, and the contents of aflatoxin B1 and benzo[a]pyrene were less than 10 μg / kg and 0.5 μg / kg, respectively.

[0025] The process also includes a resource recovery step, in which the carbon dioxide gas generated by the separation unit is condensed and liquefied and returned to the carbon dioxide supply system for recycling, with a recovery rate of not less than 95%. Meanwhile, the extraction residue is dried and pulverized for reuse as feed additives or organic fertilizers, achieving zero waste emissions throughout the entire process.

[0026] A high-efficiency extraction device for Ganoderma lucidum spore oil includes: The extraction unit consists of an extraction vessel, a carbon dioxide supply system, a pressure regulator, and a temperature controller. The extraction vessel is used to hold Ganoderma lucidum spore raw materials. The carbon dioxide supply system injects carbon dioxide into the extraction vessel through a high-pressure pump. The pressure regulator controls the extraction pressure at 20 MPa, and the temperature controller maintains the extraction temperature at 40°C. The separation unit, connected to the extraction unit via pipeline, includes a primary separator and a secondary separator. The primary separator reduces the pressure to 10 MPa to separate some carbon dioxide, and the secondary separator further reduces the pressure to 5 MPa and cools to 20°C to achieve complete extraction of Ganoderma lucidum spore oil. The purification unit includes a deacidification tank and a heavy metal removal device. The deacidification tank has a built-in stirrer and pH sensor for alkali refining treatment, and the heavy metal removal device uses a chelating resin bed. The control system is integrated with a PLC programmable logic controller to monitor extraction pressure, temperature, flow rate and purification parameters in real time, and to set and adjust process conditions through a human-machine interface.

[0027] The extraction vessel of the extraction unit adopts a double-jacket design, with circulating heat transfer oil inside the jacket. The temperature controller adjusts the temperature through a PID algorithm, with a fluctuation range not exceeding ±1℃. The extraction vessel is also equipped with a stirring paddle with a stirring speed of 50r / min. The output formula of the PID control algorithm is as follows: ; ; in This indicates the output signal of the controller. Indicates the error signal. This is the extraction temperature setting. It is a real-time monitored temperature value. Represents the proportional gain coefficient. Represents the integral gain coefficient. Represents the differential gain coefficient. Represents a time variable. It is an integral variable.

[0028] Both the primary and secondary separators of the separation unit are equipped with pressure sensors and automatic pressure relief valves. The pressure relief valves have a response time of less than 1 second. The inner walls of the separators are coated with polytetrafluoroethylene to prevent Ganoderma lucidum spore oil from adhering.

[0029] The control system's PLC programmable logic controller integrates a data acquisition module, which records extraction pressure, temperature, flow rate, and purification parameters in real time. The data is then transmitted wirelessly to a cloud server for remote monitoring and fault diagnosis. The device is also equipped with a safety interlock system that automatically shuts down the machine in case of overpressure or overtemperature.

[0030] Example 2: A high-efficiency extraction process for Ganoderma lucidum spore oil, comprising the following steps: Step 1: Pre-treatment. Select Ganoderma lucidum spore raw materials, screen them to remove impurities, and then use microwave-assisted cell wall breaking to break the spore walls. Step 2: Supercritical extraction. Place the broken Ganoderma lucidum spores in a supercritical extraction device, use carbon dioxide as the extraction solvent, control the extraction pressure at 30 MPa, the extraction temperature at 50℃, the carbon dioxide flow rate at 20 kg / h, and the extraction time at 2 hours, so that the Ganoderma lucidum spore oil dissolves in the supercritical fluid. Step 3: Separation and purification. The extracted supercritical fluid is introduced into a separator. By reducing the pressure to 8 MPa and the temperature to 25°C, carbon dioxide is vaporized and separated to obtain crude Ganoderma lucidum spore oil. The crude oil is then purified, including deacidification and heavy metal removal. Deacidification is performed by adjusting the acid value to 0.8 mg / g using an alkali refining method, and heavy metal removal is performed by chelating agent treatment. Step 4: Post-processing. The purified Ganoderma lucidum spore oil is crystallized at low temperature to remove impurities. Then, it is filtered to obtain refined Ganoderma lucidum spore oil. The peroxide value is controlled to be below 0.25g / 100g. The total triterpenoid content in the final product, calculated as oleanolic acid, is not less than 28%, and the moisture and volatile matter content is not higher than 0.1%.

[0031] In step one, the cell wall breaking process uses microwave-assisted cell wall breaking method. The microwave power is set to 400W, the processing time is 8 minutes, the cell wall breaking rate is not less than 95%, and the spore particle size after cell wall breaking is controlled at 75 micrometers.

[0032] In step two, during the supercritical extraction process, the flow rate of carbon dioxide is controlled by a mass flow meter, and an entrainer is added. The entrainer is ethanol or water, and the amount added is 8% of the mass of carbon dioxide.

[0033] Step three of the purification process also includes a microbial control step, which involves filtration using a microfiltration membrane.

[0034] In step four, the crystallization process was carried out at 0°C for 3 hours. A centrifuge was used to separate the crystallized impurities. The relative density of the product was controlled at 0.915, and the contents of aflatoxin B1 and benzo[a]pyrene were less than 10 μg / kg and 0.5 μg / kg, respectively.

[0035] The process also includes a resource recovery step, in which the carbon dioxide gas generated by the separation unit is condensed and liquefied and returned to the carbon dioxide supply system for recycling, with a recovery rate of not less than 95%. Meanwhile, the extraction residue is dried and pulverized for reuse as feed additives or organic fertilizers, achieving zero waste emissions throughout the entire process.

[0036] A high-efficiency extraction device for Ganoderma lucidum spore oil includes: The extraction unit consists of an extraction vessel, a carbon dioxide supply system, a pressure regulator, and a temperature controller. The extraction vessel is used to hold Ganoderma lucidum spore raw materials. The carbon dioxide supply system injects carbon dioxide into the extraction vessel through a high-pressure pump. The pressure regulator controls the extraction pressure at 30 MPa, and the temperature controller maintains the extraction temperature at 50°C. The separation unit, connected to the extraction unit via pipeline, includes a primary separator and a secondary separator. The primary separator reduces the pressure to 13 MPa to separate some carbon dioxide, and the secondary separator further reduces the pressure to 8 MPa and cools to 25°C to achieve complete extraction of Ganoderma lucidum spore oil. The purification unit includes a deacidification tank and a heavy metal removal device. The deacidification tank has a built-in stirrer and pH sensor for alkali refining treatment, and the heavy metal removal device uses a chelating resin bed. The control system is integrated with a PLC programmable logic controller to monitor extraction pressure, temperature, flow rate and purification parameters in real time, and to set and adjust process conditions through a human-machine interface.

[0037] The extraction vessel of the extraction unit adopts a double-jacket design, with circulating heat transfer oil inside the jacket. The temperature controller adjusts the temperature through a PID algorithm, with a fluctuation range not exceeding ±1℃. The extraction vessel is equipped with a stirring paddle with a stirring speed of 50-100r / min. The output formula of the PID control algorithm is as follows: ; ; in This indicates the output signal of the controller. Indicates the error signal. This is the extraction temperature setting. It is a real-time monitored temperature value. Represents the proportional gain coefficient. Represents the integral gain coefficient. Represents the differential gain coefficient. Represents a time variable. It is an integral variable.

[0038] Both the primary and secondary separators of the separation unit are equipped with pressure sensors and automatic pressure relief valves. The pressure relief valves have a response time of less than 1 second. The inner walls of the separators are coated with polytetrafluoroethylene to prevent Ganoderma lucidum spore oil from adhering.

[0039] The control system's PLC programmable logic controller integrates a data acquisition module, which records extraction pressure, temperature, flow rate, and purification parameters in real time. The data is then transmitted wirelessly to a cloud server for remote monitoring and fault diagnosis. The device is also equipped with a safety interlock system that automatically shuts down the machine in case of overpressure or overtemperature.

[0040] Example 3: A high-efficiency extraction process for Ganoderma lucidum spore oil, comprising the following steps: Step 1: Pre-treatment. Select Ganoderma lucidum spore raw materials, screen them to remove impurities, and then use microwave-assisted cell wall breaking to break the spore walls. Step 2: Supercritical extraction. Place the broken Ganoderma lucidum spores in a supercritical extraction device, use carbon dioxide as the extraction solvent, control the extraction pressure at 40 MPa, the extraction temperature at 60℃, the carbon dioxide flow rate at 30 kg / h, and the extraction time at 3 hours, so that the Ganoderma lucidum spore oil dissolves in the supercritical fluid. Step 3: Separation and purification. The extracted supercritical fluid is introduced into a separator. By reducing the pressure to 10 MPa and the temperature to 30°C, carbon dioxide is vaporized and separated to obtain crude Ganoderma lucidum spore oil. The crude oil is then purified, including deacidification and heavy metal removal. Deacidification is performed by adjusting the acid value to 1.0 mg / g using an alkali refining method, and heavy metal removal is performed by chelating agent treatment. Step 4: Post-processing. The purified Ganoderma lucidum spore oil is crystallized at low temperature to remove impurities. Then, it is filtered to obtain refined Ganoderma lucidum spore oil. The peroxide value is controlled to be below 0.25g / 100g. The total triterpenoid content in the final product, calculated as oleanolic acid, is not less than 28%, and the moisture and volatile matter content is not higher than 0.1%.

[0041] In step one, the cell wall breaking process adopts microwave-assisted cell wall breaking method. The microwave power is set to 500W, the processing time is 10 minutes, the cell wall breaking rate is not less than 95%, and the spore particle size after cell wall breaking is controlled at 100 micrometers.

[0042] In step two, during the supercritical extraction process, the flow rate of carbon dioxide is controlled by a mass flow meter, and an entrainer is added. The entrainer is ethanol or water, and the amount added is 10% of the mass of carbon dioxide.

[0043] Step three of the purification process also includes a microbial control step, which involves filtration using a microfiltration membrane.

[0044] In step four, the crystallization process was carried out at 5°C for 4 hours. A centrifuge was used to separate the crystallized impurities. The relative density of the product was controlled at 0.920, and the contents of aflatoxin B1 and benzo[a]pyrene were less than 10 μg / kg and 0.5 μg / kg, respectively.

[0045] The process also includes a resource recovery step, in which the carbon dioxide gas generated by the separation unit is condensed and liquefied and returned to the carbon dioxide supply system for recycling, with a recovery rate of not less than 95%. Meanwhile, the extraction residue is dried and pulverized for reuse as feed additives or organic fertilizers, achieving zero waste emissions throughout the entire process.

[0046] A high-efficiency extraction device for Ganoderma lucidum spore oil includes: The extraction unit consists of an extraction vessel, a carbon dioxide supply system, a pressure regulator, and a temperature controller. The extraction vessel is used to hold Ganoderma lucidum spore raw materials. The carbon dioxide supply system injects carbon dioxide into the extraction vessel through a high-pressure pump. The pressure regulator controls the extraction pressure at 40 MPa, and the temperature controller maintains the extraction temperature at 60°C. The separation unit, connected to the extraction unit via pipeline, includes a primary separator and a secondary separator. The primary separator reduces the pressure to 15 MPa to separate some carbon dioxide, and the secondary separator further reduces the pressure to 10 MPa and cools to 30°C to achieve complete extraction of Ganoderma lucidum spore oil. The purification unit includes a deacidification tank and a heavy metal removal device. The deacidification tank has a built-in stirrer and pH sensor for alkali refining treatment, and the heavy metal removal device uses a chelating resin bed. The control system is integrated with a PLC programmable logic controller to monitor extraction pressure, temperature, flow rate and purification parameters in real time, and to set and adjust process conditions through a human-machine interface.

[0047] The extraction vessel of the extraction unit adopts a double-jacket design, with circulating heat transfer oil inside the jacket. The temperature controller adjusts the temperature through a PID algorithm, with a fluctuation range not exceeding ±1℃. The extraction vessel is also equipped with a stirring paddle with a stirring speed of 100r / min. The output formula of the PID control algorithm is as follows: ; ; in This indicates the output signal of the controller. Indicates the error signal. This is the extraction temperature setting. It is a real-time monitored temperature value. Represents the proportional gain coefficient. Represents the integral gain coefficient. Represents the differential gain coefficient. Represents a time variable. It is an integral variable.

[0048] Both the primary and secondary separators of the separation unit are equipped with pressure sensors and automatic pressure relief valves. The pressure relief valves have a response time of less than 1 second. The inner walls of the separators are coated with polytetrafluoroethylene to prevent Ganoderma lucidum spore oil from adhering.

[0049] The control system's PLC programmable logic controller integrates a data acquisition module, which records extraction pressure, temperature, flow rate, and purification parameters in real time. The data is then transmitted wirelessly to a cloud server for remote monitoring and fault diagnosis. The device is also equipped with a safety interlock system that automatically shuts down the machine in case of overpressure or overtemperature.

[0050] Comparative Example 1: The difference between this comparative example and Example 1 is that this comparative example did not undergo cell wall breaking treatment before supercritical extraction, and directly extracted the Ganoderma lucidum spore raw material.

[0051] Comparative Example 2 differs from Example 1 in that: in the supercritical extraction process, carbon dioxide is not used as a solvent in this comparative example, but hexane is used as the extraction solvent, and extraction is carried out at atmospheric pressure and 60°C for 3 hours.

[0052] Comparative Example 3 differs from Example 1 in that: in the separation and purification steps, this comparative example did not perform deacidification and heavy metal removal treatment, but directly performed post-processing on the crude oil.

[0053] Comparative Example 4 differs from Example 1 in that no entrainer was added during the supercritical extraction process; only pure carbon dioxide was used for extraction.

[0054] The performance of the Ganoderma lucidum spore oils prepared in Examples 1-3 and Comparative Examples 1-4 was tested. The test items and test methods are as follows: The total triterpenoid content was determined by oleanolic acid, and the absorbance was measured at a wavelength of 510 nm using ultraviolet-visible spectrophotometry to calculate the oleanolic acid equivalent. For acid value testing, potassium hydroxide titration method is used. Weigh the oil sample, dissolve it in neutral ethanol-ether mixture, use phenolphthalein as indicator, titrate with standard potassium hydroxide solution to the endpoint, and calculate the number of milligrams of potassium hydroxide required for free fatty acids per gram of oil. The peroxide value was tested using the sodium thiosulfate titration method. The oil sample was dissolved in a mixture of glacial acetic acid and chloroform, potassium iodide solution was added, and after reacting in the dark, it was titrated with standard sodium thiosulfate solution to calculate the peroxide content per 100 grams of oil. For heavy metal content testing, inductively coupled plasma mass spectrometry was used. After microwave digestion, the oil sample was injected into the ICP-MS instrument to detect the content of lead, arsenic, mercury, and cadmium, and the total amount was calculated.

[0055] Table 1. Comprehensive performance test data of Ganoderma lucidum spore oil prepared in Examples 1-3 and Comparative Examples 1-4: By comparing and analyzing the data in the table, it can be seen that the Ganoderma lucidum spore oil prepared using the processes in Examples 1-3 has significantly better performance than the Ganoderma lucidum spore oil prepared using the processes in Comparative Examples 1-4. This indicates that the present invention, by adding a pretreatment device containing a microwave cell-wall breaking unit, performs efficient cell-wall breaking treatment on the Ganoderma lucidum spore raw material, destroying the dense structure of the spore wall, making the internal oil easier to release, thereby improving the extraction efficiency and the yield of the target product in subsequent extraction processes; by using an extraction system based on supercritical carbon dioxide and synergistically using an entrainer, it utilizes… By utilizing the unique high diffusivity and strong solubility of supercritical fluids, combined with the solubilizing effect of entrainers on polar components, efficient and selective extraction of lipid-soluble and some polar active components from Ganoderma lucidum spores is achieved, improving the extraction rate and the overall quality of the extracted product. Through a purification device integrating deacidification and heavy metal removal units, the crude oil obtained from the extraction undergoes multi-stage tandem purification treatment to remove free fatty acids and potential heavy metal impurities, optimize the color, acid value, and hygiene and safety indicators of the spore oil, and finally obtain a high-purity, high-quality Ganoderma lucidum spore oil product.

[0056] By comparing and analyzing all the relevant data in Table 1, it can be seen that the Ganoderma lucidum spore oil prepared by the extraction process of the present invention has a high total triterpenoid content, a low acid value and peroxide value, and a low heavy metal content.

[0057] Table 2. Effect of different cell wall disruption times on cell wall disruption rate: Table 2 shows the effects of different cell wall disruption times on the cell wall disruption rate and spore oil yield of Ganoderma lucidum spores. As the disruption time increases, the disruption rate initially rises rapidly, reaching 91.8% when the disruption time reaches 20 minutes. Further extending the disruption time to 25 minutes causes the increase in disruption rate to slow down.

[0058] Table 3. Effect of different extraction pressures on extraction rate: Table 3 shows the effect of different extraction pressures on the extraction rate and content of major active ingredients of Ganoderma lucidum spore oil. With increasing extraction pressure, the extraction rate gradually increased, reaching 31.2% at 30 MPa. Further increasing the pressure to 35 MPa did not significantly increase the extraction rate.

[0059] Table 4. Effect of different extraction temperatures on extraction efficiency: Table 4 reflects the effects of different extraction temperatures on the extraction rate and extraction time of Ganoderma lucidum spore oil. As the temperature increases, the extraction rate initially increases and then decreases, reaching a maximum of 32.5% at 50℃, at which point the extraction time is 60 minutes. Excessively high temperatures can lead to the loss of heat-sensitive components.

[0060] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Without further limitations, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes said element.

[0061] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A highly efficient extraction process for Ganoderma lucidum spore oil, characterized in that: The process comprises the following steps: Step one: pretreatment, select ganoderma spore raw materials, remove impurities by screening, then use microwave assisted wall breaking to break the wall, so that the spore wall is broken; Step two: supercritical extraction, place the broken wall ganoderma spores in the supercritical extraction device, use carbon dioxide as the extraction solvent, control the extraction pressure at 20-40 MPa, the extraction temperature at 40-60 ℃, the carbon dioxide flow at 10-30 kg / h, and the extraction time at 1-3 hours, so that the ganoderma spore oil is dissolved in the supercritical fluid; Step three: separation and purification, the extracted supercritical fluid is introduced into the separator, the carbon dioxide is separated by reducing the pressure to 5-10 MPa and the temperature to 20-30 ℃, and the crude ganoderma spore oil is obtained, then the crude oil is purified, including the steps of deacidification and heavy metal removal, wherein the deacidification uses alkali refining method to adjust the acid value to 0.5-1.0 mg / g, and the heavy metal removal is treated by chelating agent; Step four: post-treatment, the purified ganoderma spore oil is crystallized under low temperature conditions to precipitate impurities, then filtered to obtain refined ganoderma spore oil, and the peroxide value is controlled below 0.25 g / 100 g, the total triterpenoid content in the final product is not less than 28% calculated by oleanolic acid, and the moisture and volatile matter content is not higher than 0.1%.

2. The process as claimed in claim 1, wherein the process is characterized by: The wall breaking treatment in step one uses microwave assisted wall breaking method, the microwave power is set to 300-500 W, the treatment time is 5-10 minutes, the wall breaking rate is not less than 95%, and the spore particle size after wall breaking is controlled within 50-100 microns.

3. The process as claimed in claim 1, wherein the process is characterized by: In the supercritical extraction process of step two, the flow of carbon dioxide is controlled by a mass flow meter, and a entrainer is added, the entrainer is ethanol or water, and the addition amount is 5-10% of the mass of carbon dioxide.

4. The process as claimed in claim 1, wherein the process is characterized by: The purification treatment in step three also includes a microorganism control step, which is filtered by a microfiltration membrane.

5. The process as claimed in claim 1, wherein the process is characterized by: The crystallization treatment in step four is carried out at-5 to 5 ℃, the crystallization time is 2-4 hours, and the crystallization impurities are separated by a centrifuge, the relative density of the product is controlled within 0.910-0.920, and the contents of aflatoxin B1 and benzopyrene are less than 10 μg / kg and 0.5 μg / kg respectively.

6. The process as claimed in claim 1, wherein the process is characterized by: The process also includes a resource recovery step, the carbon dioxide gas generated by the separation unit is liquefied by condensation and then returned to the carbon dioxide supply system for recycling, the recovery rate is not less than 95%; At the same time, the extraction residue is treated by drying and crushing, and reused as a feed additive or organic fertilizer.

7. A high-efficiency extraction device for Ganoderma lucidum spore oil, used to realize the high-efficiency extraction process of Ganoderma lucidum spore oil according to any one of claims 1-6, characterized in that: It comprises: An extraction unit composed of an extraction kettle, a carbon dioxide supply system, a pressure regulator and a temperature controller, the extraction kettle is used to contain ganoderma spore raw materials, the carbon dioxide supply system injects carbon dioxide into the extraction kettle through a high-pressure pump, the pressure regulator controls the extraction pressure within 20-40 MPa, and the temperature controller maintains the extraction temperature at 40-60 ℃; The separation unit is connected with the extraction unit through a pipeline, and comprises a first separator and a second separator. The first separator separates part of the carbon dioxide by reducing the pressure to 10-15 MPa. The second separator further reduces the pressure to 5-10 MPa and the temperature to 20-30 DEG C, so that the ganoderma spore oil is completely separated out. The purification unit comprises a deacidification tank and a heavy metal removal device. The deacidification tank is provided with a stirrer and a pH sensor, and is used for alkali refining treatment. The heavy metal removal device adopts a chelating resin bed. The control system is integrated with a PLC programmable logic controller, and real-time monitoring of the extraction pressure, temperature, flow rate and purification parameters is performed. The process conditions are set and adjusted through a human-machine interface.

8. The high-efficiency ganoderma spore oil extraction device according to claim 7, characterized in that: The extraction kettle of the extraction unit adopts a double-layer jacket design. Circulating heat-conducting oil is circulated in the jacket. A temperature controller adjusts the temperature through a PID algorithm. The fluctuation range is not more than ±1 DEG C. The extraction kettle is provided with a stirring paddle. The stirring speed is 50-100 r / min. The output formula of the PID control algorithm is as follows: ； ； wherein represents an output signal of the controller, represents an error signal, is an extraction temperature set value, is a real-time monitored temperature value, represents a proportional gain coefficient, represents an integral gain coefficient, represents a differential gain coefficient, represents a time variable, is an integral variable.

9. The high-efficiency ganoderma spore oil extraction device according to claim 7, characterized in that: The first separator and the second separator of the separation unit are both provided with a pressure sensor and an automatic pressure relief valve. The response time of the pressure relief valve is less than 1 second. The inner wall of the separator is coated with a polytetrafluoroethylene coating to prevent the ganoderma spore oil from adhering.

10. The high-efficiency ganoderma spore oil extraction device according to claim 7, characterized in that: The PLC programmable logic controller of the control system is integrated with a data acquisition module. The extraction pressure, temperature, flow rate and purification parameters are recorded in real time. The data are transmitted to a cloud server through wireless transmission, so that remote monitoring and fault diagnosis are realized. Meanwhile, the device is provided with a safety interlocking system. The device is automatically stopped when the pressure or temperature is too high.

Images