CN115141679B - Ganoderma lucidum spore oil with natural flavor - Google Patents
Ganoderma lucidum spore oil with natural flavor Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/12—Refining fats or fatty oils by distillation
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
Abstract
The invention belongs to the field of natural product extraction and traditional Chinese medicine preparation, and relates to ganoderma lucidum spore oil with natural flavor. The pressure and temperature of the extraction kettle and the rectification column can be regulated in the preparation process, and the ganoderma lucidum spore oil with different specifications and flavors can be obtained. The ganoderma lucidum spore oil is used as a carrier of the volatile oil, so that the loss of the volatile oil is greatly reduced, and simultaneously, the ganoderma lucidum spore oil with natural flavor in various specifications is obtained. The quality and stability of the extract of other natural products obtained by extraction are superior to those of the conventional extract, the comprehensive utilization of other natural products is realized, and the extract can be used as raw materials of foods, health-care foods or cosmetics. The invention can perform supercritical combined extraction and rectification purification on line.
Description
Technical Field
The invention belongs to the field of natural product extraction and traditional Chinese medicine preparation, relates to the technical field of processing and utilization of ganoderma lucidum spores, and in particular relates to ganoderma lucidum spore oil with natural flavor.
Background
Ganoderma Ganoderma lucidum (Leys. ExFr.) Karst or Ganoderma Ganoderma sinense Zhao, xu et Zhang is dry fruiting body of Ganoderma lucidum of Polyporaceae (part 2020 of Chinese pharmacopoeia), has mild taste and is effective in strengthening body resistance and consolidating constitution. The Ganoderma spore powder is collection of Ganoderma spore of germ cells generated in mature period of Ganoderma fruiting body. Contains unsaturated fatty acids, sterols, triterpenes, alkaloids, lactones, proteins and amino acids, glycopeptides and inorganic salts. The ganoderma lucidum spore oil is extracted from ganoderma lucidum spore powder, is rich in active ingredients of the ganoderma lucidum spore powder, is easy to be absorbed and utilized by human bodies, and modern researches show that the ganoderma lucidum spore oil is rich in triterpene compounds, sterols and unsaturated fatty acids, and has higher application values in the aspects of nerve regulation, immune regulation, anti-tumor, liver protection, blood lipid reduction and the like.
The volatile oil extracted from natural plants is also called plant essential oil, is a generic term of oily liquid which can volatilize along with steam distillation and is not mixed with water at normal temperature, and has the effects of dispersing and relieving exterior syndrome, inducing resuscitation with aromatics, regulating qi to alleviate pain, dispelling wind and removing dampness, activating blood and dissolving stasis, dispelling cold and warming interior, clearing heat and detoxicating, relieving summer heat and removing dirt, killing parasites and resisting bacteria, such as angelica oil and bupleurum oil, etc. Volatile oil is an important raw material in medicine, food and cosmetics. The volatile oil contains more chemical components, and the volatile oil extraction method comprises a steam distillation method and an organic solvent extraction method, but the traditional extraction method is easy to cause partial unstable aroma components to be heated and deteriorated or have solvent residues, thereby influencing the aroma and the quality of the product.
The supercritical carbon dioxide extraction technology refers to that carbon dioxide is contacted with a substance to be separated in a supercritical state, and the components with polarity, boiling point and molecular weight are extracted in sequence by controlling the change of critical pressure and critical temperature. Meanwhile, the density, polarity and dielectric constant of the supercritical carbon dioxide are increased along with the increase of the closed critical pressure, and components with different polarities can be extracted step by utilizing the boosting. The mixed components are obtained by controlling the conditions, then the solubility of the supercritical carbon dioxide to the extracted substances is reduced by means of decompression and temperature rising and falling, and the extracted substances are automatically and completely separated out, so that the aim of separation and purification is fulfilled, and the extraction and separation processes are integrated.
As shown in figure 1, the conventional supercritical separation equipment comprises an extraction kettle I1-1, a separation kettle I2-2, a separation kettle II 2-3, a heat exchanger I3-1, a storage tank 4, a high-pressure pump 5 and a heat exchanger II 3-2 which are sequentially connected through pipelines, wherein the heat exchanger II 3-2 is connected with the extraction kettle I to form closed loop connection, a valve V2 and a trimming valve F1 are arranged on a connecting pipeline between the extraction kettle I1-1 and the separation kettle I2-2, a trimming valve F2 is arranged on a pipeline between the separation kettle I2-2 and the separation kettle II, a valve V3 is arranged between the separation kettle II and the heat exchanger I3-1, a valve V4 is arranged between the storage tank 4 and the high-pressure pump 5, a valve V5 is arranged between the high-pressure pump 5 and the heat exchanger II 3-2, a collecting valve C1 is arranged below the separation kettle I2-2, and a collecting valve C2 is arranged below the separation kettle II.
The current supercritical technology has some defects: 1, during conventional supercritical carbon dioxide extraction, carbon dioxide in a supercritical state not only extracts ganoderma lucidum spore oil and volatile oil of other natural products, but also extracts a large amount of fat-soluble impurities and residual moisture together, so that the valence of the separated ganoderma lucidum spore oleic acid is increased, the peroxide value is increased, the appearance is turbid, and the quality is reduced. 2, as shown in figure 1, in the conventional supercritical carbon dioxide extraction, the pressure-increasing sequence after the supercritical carbon dioxide enters the system is an extraction kettle I, a separation kettle I and a separation kettle II. When supercritical carbon dioxide enters a separation kettle I, the pressure of the separation kettle I does not reach a set value in time, so that fat-soluble impurities and water carried by the supercritical carbon dioxide are not brought to a separation kettle II in time, the supercritical carbon dioxide is separated and settled at the bottom of the separation kettle I, pollution is caused, and spore oil in 1h after separation begins is required to be discarded; when separation is carried out, as the separation stroke of the conventional separation kettle I is shorter, the length of the separation kettle is that the diameter=4-5:1, and part of qualified ganoderma lucidum spore oil and volatile oil are not fully separated from carbon dioxide in the separation kettle I and are brought to the separation kettle II, so that waste is caused. And 3, the content of volatile oil in most natural products is lower and is about less than 1% of the weight of the materials, the volatile oil obtained by conventional supercritical separation is easy to adhere to the separation kettle wall and the connecting pipeline, is difficult to collect and use, and the yield is lower.
The supercritical carbon dioxide rectification is to selectively extract a target product by changing the density of the supercritical carbon dioxide according to a variable temperature reflux principle so as to change the dissolving capacity of the supercritical carbon dioxide on the extract components. The rectification can lead the mixture to be more completely separated, and the key is reflux caused by temperature difference: the components with low boiling points in the spore oil and the essential oil are continuously carried to a later separation kettle by supercritical carbon dioxide along with the temperature rise, and the components with high boiling points in the spore oil and the essential oil are gradually deposited at the bottom of the rectifying column, so that relatively pure component products with different boiling points are respectively obtained at the two ends of the rectifying column.
Patent CN201310272711.X A ganoderma lucidum and ginseng composite extract and preparation method and application thereof are used for 1: 10-10: 1 weight ratio of Ganoderma and Ginseng radix, mixing to obtain composite powder, and supercritical CO 2 The invention mixes materials before extracting, and the materials of the ganoderma lucidum and the ginseng are difficult to separate after extracting and can be used once, thus causing waste; during extraction, adding 85% ethanol entrainer, introducing organic solvent, and carrying out solvent residue risk; the yield of the compound oil obtained after extraction is low, and is only 1.6% at maximum, so that the large-scale production is difficult to industrialize.
Patent CN201110001099.3 is a multi-body multistage supercritical C0 2 The method for extracting the ganoderma lucidum spore oil is characterized in that a rectifying device and a multi-gradient temperature and pressure regulating and separating system are additionally arranged in a separating kettle device, so that triterpene substances with various chemical structures and wider polarities in the ganoderma lucidum spore oil are extracted, 90% ethanol serving as an entrainer is added, and an organic solvent is introduced; in order to effectively separate ethanol and water from ganoderma lucidum spore oil, multi-body and multi-stage separation is used, and the method is complex and high in production cost.
At present, the ganoderma lucidum spore oil has the advantage of being gradually accepted by people, but the taste of the ganoderma lucidum spore oil is very little, so that the crowd actively eating the ganoderma lucidum spore oil can expand various user groups by adding natural flavors of various flowers into the ganoderma lucidum spore oil.
Disclosure of Invention
The invention aims to provide the ganoderma lucidum spore oil with higher quality and natural flavor, so that people can more easily accept the ganoderma lucidum spore oil and products thereof, and the extraction yield of volatile oil in natural products is improved.
The glossy ganoderma spore oil with natural flavor is prepared through supercritical carbon dioxide combined extraction to extract glossy ganoderma spore oil from glossy ganoderma spore powder and volatile oil from other natural products, variable temperature and pressure rectification and mixing volatile oil with glossy ganoderma spore oil as carrier.
The invention creatively solves the defects of high price, high peroxide value, turbid appearance and reduced quality of the ganoderma lucidum spore oleic acid obtained by separation caused by extracting a large amount of fat-soluble impurities and residual moisture together in the conventional supercritical carbon dioxide extraction by a temperature-changing pressure rectification mode, and simultaneously fully mixes volatile oil in other natural products in the rectification process by taking ganoderma lucidum spore oil with high extraction rate as a carrier, thereby improving the extraction yield of the volatile oil in the natural products.
The supercritical carbon dioxide combined extraction technology refers to: during supercritical extraction, the ganoderma lucidum spore powder and other natural products are extracted in different extraction kettles at the same time, and the lipid-soluble components of the ganoderma lucidum spore powder and the lipid-soluble components of other natural products dissolved in the carbon dioxide under the supercritical state are conveyed to a rectifying column.
The invention purifies fat-soluble components with impurities through the rectifying column so as to ensure the quality of finished products.
The temperature-changing pressure-changing rectification technology refers to that under the temperature and pressure regulation of a rectification column, the solubility of ganoderma lucidum spore oil and volatile oil of carbon dioxide dissolved in a supercritical state is reduced due to pressure change, so that the ganoderma lucidum spore oil and the volatile oil are separated; purifying by temperature difference change of temperature change section of rectifying column, mixing volatile oil with Ganoderma spore oil as carrier, and removing impurities. Volatile oil and other fat-soluble impurities in other natural products are separated through variable-temperature and variable-pressure rectification, the volatile oil and the ganoderma lucidum spore oil obtained through separation are uniformly mixed, so that the ganoderma lucidum spore oil with clear appearance and natural flavor is formed, working hours and energy consumption are saved, a finished product is selected through temperature and pressure control, and quality control is performed.
The unique extraction process of the fat-soluble component of the ganoderma lucidum spore powder and the volatile oil component in other natural products is as follows: collecting mature Ganoderma spore, collecting into powder, sieving to remove impurities, breaking wall, granulating, oven drying to water content below 3%, collecting wall-broken Ganoderma spore powder particles, adding into extraction kettle II of supercritical extraction device, sealing, sequentially introducing carbon dioxide from separation kettle-rectifying column-extraction kettle II-extraction kettle I, and performing supercritical extraction after rectifying column reaches preset pressure and temperature: the pressure of the extraction kettle II is 20-25 MPa, and the extraction temperature is 40-50 ℃; collecting other natural products, sieving to remove impurities, grinding, granulating, oven drying until the water content is below 3%, taking other natural products with certain weight, putting into an extraction kettle I of a supercritical extraction device, sealing, introducing supercritical carbon dioxide, and performing supercritical extraction: the pressure of the extraction kettle I is 20-25 MPa, the extraction temperature is 40-50 ℃, the combined extraction of the wall-broken ganoderma lucidum spore powder and other natural products is carried out simultaneously or at intervals, the extraction kettle II and the extraction kettle I can extract ganoderma lucidum spore oil with different specifications from the wall-broken ganoderma lucidum spore powder and other natural products under different pressures and temperatures, the flow rate during the extraction is 110-120L/h, and the extraction time is 2-3 h.
Firstly, introducing supercritical carbon dioxide in sequence, filling the separation kettle, the rectifying column and the extraction kettle with carbon dioxide, and raising the pressure and temperature of the separation kettle, the rectifying column and the extraction kettle in sequence, so that volatile oil and other fat-soluble impurities in ganoderma lucidum spore oil and other natural products are separated in the rectifying column in time when extraction starts, and subsequent pollution is avoided. The pressure of the rectifying column is timely reduced during variable-temperature and variable-pressure rectification, the separation efficiency is improved, the working hours and the energy consumption are saved, and the mixing proportion of the volatile oil in the spore oil and other natural products is stabilized.
The separation process of volatile oil components in ganoderma lucidum spore oil and other natural products comprises the following steps: when the combined extraction of the wall-broken ganoderma lucidum spore powder and other natural products is started, the extraction pressure of a rectifying column is 8-12 MPa, the rectifying column is divided into a plurality of variable temperature sections, the temperature is 35-50 ℃, the temperature of each section is different, the length of the rectifying column is that the diameter=30:1, the rectifying column is filled with filler, the filler is made of stainless steel or ceramic, and ganoderma lucidum spore oil with different flavors is collected from the rectifying column under different pressures and temperatures.
The pressure change is that the pressure is changed from high to low. As the pressure decreases, the solubility of the mixed oil in the carbon dioxide in the rectification column decreases and the mixed oil precipitates.
The rectifying column is divided into four sections, a temperature changing section T1=35 ℃, a temperature changing section T2=40 ℃, a temperature changing section T3=45 ℃ and a temperature changing section T4=50 ℃.
The flavor component of the ganoderma lucidum spore oil with natural flavor can exist stably for more than or equal to 6 months at the ambient temperature of less than or equal to 37 ℃.
The Ganoderma is Polyporaceae fungus Ganoderma lucidum (Ganoderma lucidum (Leyss. ExFr.) karst.) or Ganoderma sinense (Ganoderma sinense Zhao, xu et Zhang)
The technical scheme adopted by the invention adopts careful process design, and the experiment is repeated for a plurality of times, and adopts specific process parameters, so that the method has the beneficial effects that:
1, simultaneously extracting the ganoderma lucidum spore oil and the volatile oil of other natural products by supercritical carbon dioxide, saving working hours and energy consumption, and selectively adjusting the proportion of the ganoderma lucidum spore oil and the volatile oil of other natural products by different feeding amounts, pressures, temperatures and times of different extraction kettles to obtain the ganoderma lucidum spore oil with natural flavor of different specifications.
2, separating the ganoderma lucidum spore oil and other fat-soluble impurities through variable-temperature and variable-pressure rectification, and separating to obtain the ganoderma lucidum spore oil with clear appearance, wherein the acid value and the peroxide value are lower than the national standard of edible oil and are also lower than those of ganoderma lucidum spore oil obtained by a conventional supercritical technology. Volatile oil and other fat-soluble impurities in other natural products are separated through variable-temperature and variable-pressure rectification, and the volatile oil and the ganoderma lucidum spore oil obtained through separation are uniformly mixed to form the ganoderma lucidum spore oil with clear appearance and natural flavor, so that the working time and the energy consumption are saved.
3, when supercritical carbon dioxide is combined with extraction, namely variable-temperature and variable-pressure rectification, the separation kettle, the rectification column and the extraction kettle are firstly boosted and heated in sequence, so that the volatile oil and other fat-soluble impurities in the ganoderma lucidum spore oil and other natural products are timely separated in the rectification column when the extraction is started, and the subsequent pollution is avoided. The pressure of the rectifying column is timely reduced during variable-temperature and variable-pressure rectification, the separation efficiency is improved, the working hours and the energy consumption are saved, and the mixing proportion of the volatile oil in the spore oil and other natural products is stabilized.
4, the supercritical carbon dioxide combined extraction-variable-temperature and variable-pressure rectification technology solves the defects that the volatile oil content in other natural products is too low, the volatile oil obtained through supercritical separation is easy to adhere to the separation kettle wall, and the volatile oil is difficult to collect and utilize. The ganoderma lucidum spore oil is used as a carrier of the volatile oil, so that the loss of the volatile oil is greatly reduced, and simultaneously, the ganoderma lucidum spore oil with natural flavor in various specifications is obtained.
5, the whole process temperature of the supercritical carbon dioxide combined extraction-variable temperature and pressure rectification technology is controllable, the extraction and separation temperature is not higher than the denaturation temperature of volatile oil in other natural products, the quality of the ganoderma lucidum spore oil with natural flavor obtained by separation is stable, and the stable existence time of the flavor components is not less than 6 months under the condition that the ambient temperature is not more than 37 ℃.
6, the supercritical carbon dioxide combined extraction-variable temperature and pressure rectification technology uses food-grade carbon dioxide as an extraction carrier, so that the method is environment-friendly, and saves labor hour and energy consumption. The processing process has no entrainer, avoids organic solvent pollution, and the obtained ganoderma lucidum spore oil with natural flavor can pass through organic authentication, can be prepared into a preparation by adding auxiliary materials which are permitted by the organic authentication, and can be authenticated as an organic product.
7, removing fat-soluble components from other natural product components remained after supercritical carbon dioxide combined extraction, and further extracting. The quality and stability of the extract of other natural products obtained by extraction are superior to those of the conventional extract, and the comprehensive utilization of other natural products is realized: 1, the glossy ganoderma fruiting body after extracting fat-soluble components is extracted by water or alcohol, the extract can be directly dried into powder, auxiliary materials such as dextrin and the like are not needed to be added in the conventional glossy ganoderma extract, and the hygroscopicity is greatly reduced compared with the conventional glossy ganoderma extract. 2, extracting the American ginseng particles with water or alcohol to obtain an American ginseng extract after extracting fat-soluble components, and mixing the American ginseng extract with the American ginseng volatile oil obtained by the original supercritical carbon dioxide extraction to obtain the American ginseng extract with the American ginseng flavor, thereby avoiding unnecessary loss of the flavor in the American ginseng raw material during conventional extraction and concentration.
Drawings
FIG. 1 is a schematic diagram of a conventional supercritical extraction separation apparatus
FIG. 2 is a schematic diagram of a supercritical combined extraction-variable temperature and pressure swing rectification purification separation apparatus according to an embodiment of the present invention wherein: 1-1, an extraction kettle I; 1-2, an extraction kettle II; 2-1, a rectifying column and a temperature changing section T1-a temperature changing section T4;2-2, separating kettle I; 2-3, separating kettle II; 3-1, a heat exchanger I; 3-2, a heat exchanger II; 4. a storage tank; 5. a high pressure pump; fine tuning valve F1, fine tuning valve F2, collection valve C1, collection valve C2, valve V1-valve V7.
Detailed Description
The following examples further illustrate the invention but are not to be construed as limiting the invention and modifications or alternatives to the methods, steps or conditions of the invention are within the scope of the invention without departing from the spirit and nature of the invention.
A ganoderma lucidum spore oil with natural flavor is prepared by the following steps: extracting volatile oil from Ganoderma spore oil and other natural products from Ganoderma spore powder by supercritical carbon dioxide combined extraction, rectifying at variable temperature and pressure, and mixing volatile oil with Ganoderma spore oil as carrier.
The supercritical carbon dioxide combined extraction technology refers to: during supercritical extraction, the ganoderma lucidum spore powder and other natural products are extracted in different extraction kettles at the same time, and the lipid-soluble components of the ganoderma lucidum spore powder and the lipid-soluble components of other natural products dissolved in the carbon dioxide under the supercritical state are conveyed to a rectifying column. Under the temperature and pressure regulation of the rectifying column, the solubility of the ganoderma lucidum spore oil and the volatile oil of the carbon dioxide dissolved in the supercritical state is reduced due to the pressure change, so that the ganoderma lucidum spore oil and the volatile oil are separated; purifying by temperature difference change of temperature change section of rectifying column, mixing volatile oil with Ganoderma spore oil as carrier, and removing impurities.
The unique extraction process of the fat-soluble component of the ganoderma lucidum spore powder and the volatile oil component in other natural products is as follows: collecting mature ganoderma lucidum spores, collecting the ganoderma lucidum spores into powder, sieving to remove impurities, breaking wall, granulating, drying until the moisture is below 3%, then taking wall-broken ganoderma lucidum spore powder particles with a certain weight, putting the wall-broken ganoderma lucidum spore powder particles into an extraction kettle II of a supercritical extraction device, sealing, sequentially introducing carbon dioxide from a separation kettle II-rectifying column-an extraction kettle II-an extraction kettle I, and performing supercritical extraction after the rectifying column reaches a set pressure and temperature: the pressure of the extraction kettle II is 20-25 MPa, and the extraction temperature is 40-50 ℃; collecting other natural products, sieving to remove impurities, grinding, granulating, oven drying until the water content is below 3%, taking other natural products with certain weight, putting into an extraction kettle I of a supercritical extraction device, sealing, introducing supercritical carbon dioxide, and performing supercritical extraction: the pressure of the extraction kettle I is 20-25 MPa, the extraction temperature is 40-50 ℃, the combined extraction of the wall-broken ganoderma lucidum spore powder and other natural products is carried out simultaneously or at intervals, the extraction kettle II and the extraction kettle I can extract ganoderma lucidum spore oil with different specifications from the wall-broken ganoderma lucidum spore powder and other natural products under different pressures and temperatures, the flow rate during the extraction is 110-120L/h, and the extraction time is 2-3 h.
Firstly, introducing supercritical carbon dioxide in sequence, filling the separation kettle, the rectifying column and the extraction kettle with carbon dioxide, and raising the pressure and temperature of the separation kettle, the rectifying column and the extraction kettle in sequence, so that volatile oil and other fat-soluble impurities in ganoderma lucidum spore oil and other natural products are separated in the rectifying column in time when extraction starts, and subsequent pollution is avoided. The pressure of the rectifying column is timely reduced during variable-temperature and variable-pressure rectification, the separation efficiency is improved, the working hours and the energy consumption are saved, and the mixing proportion of the volatile oil in the spore oil and other natural products is stabilized.
The separation process of volatile oil components in ganoderma lucidum spore oil and other natural products comprises the following steps: when the combined extraction of the wall-broken ganoderma lucidum spore powder and other natural products is started, the extraction pressure of a rectifying column is 8-12 MPa, the rectifying column is divided into a plurality of variable temperature sections, the temperature is 35-50 ℃, the temperature of each section is different, the length of the rectifying column is that the diameter=30:1, the rectifying column is filled with filler, the filler is made of stainless steel or ceramic, and ganoderma lucidum spore oil with different flavors is collected from the rectifying column under different pressures and temperatures.
The pressure change is that the pressure is changed from high to low. As the pressure decreases, the solubility of the mixed oil in the carbon dioxide in the rectifying column is reduced, the rectifying column is divided into four sections, the temperature change section t1=35 ℃, the temperature change section t2=40 ℃, the temperature change section t3=45 ℃, and the temperature change section t4=50 ℃.
Example 1
A method for extracting volatile oil from fruiting body of Ganoderma lucidum by conventional supercritical extraction and separation equipment (shown in figure 1) comprises the following steps: preparing volatile oil of ganoderma lucidum fruiting body: harvesting mature ganoderma lucidum fruiting bodies, screening impurities, drying until the moisture is below 3%, grinding into particles, marking the particles as a raw material I, taking 7kg, putting into an extraction kettle I1-1 of a supercritical extraction device, sealing, opening a valve V1-valve V5, closing fine tuning valves F1 and F2, introducing supercritical carbon dioxide, and performing supercritical extraction: when the pressure of the extraction kettle I is 25MPa, the fine tuning valve F1 is opened when the temperature of the extraction kettle I is 45 ℃, the pressure and the temperature of the extraction kettle I are kept, supercritical carbon dioxide is introduced into the separation kettle I2-2, the pressure of the separation kettle I is 8MPa, the fine tuning valve F2 is opened when the temperature is 50 ℃, the pressure and the temperature of the separation kettle I are kept, supercritical carbon dioxide is introduced into the separation kettle II 2-3, the pressure of the separation kettle II is 5.5MPa, the temperature is 50 ℃, the flow rate is 110-120L/h, the extraction time is 5h, after the extraction is finished, the fine tuning valves F1, F2 and the valve V3 are closed, carbon dioxide in the separation kettles I and II are discharged by the collecting valves C1 and C2, the upper covers of the separation kettles I and II are opened after the air pressure is reduced to 0.1MPa, about 35g of ganoderma lucidum fruit body volatile oil I is obtained from the wall scraping of the separation kettle I, no oil is collected from the separation kettle II, and the appearance of ganoderma lucidum fruit body volatile oil I is slightly turbid. After the extraction is completed, the ganoderma lucidum fruiting body particles in the extraction kettle I are taken out and weighed to obtain ganoderma lucidum fruiting body particles of about 6.8kg, which means that the raw material I contains about 200g of fat-soluble components to be extracted. However, only about 35g of volatile oil of the fruiting body of ganoderma lucidum is obtained.
A method for extracting Ganoderma spore oil by conventional supercritical extraction separation equipment (figure 1) comprises the following steps: preparation of ganoderma lucidum spore oil: collecting mature ganoderma spores, collecting the ganoderma spores into powder, sieving to remove impurities, drying until the moisture is less than 3%, breaking the wall, granulating, marking the ganoderma spores as a raw material II, taking 7kg of ganoderma spores, putting the ganoderma spores into an extraction kettle of a supercritical extraction device, sealing, opening a valve V1-a valve V5, closing fine tuning valves F1 and F2, introducing supercritical carbon dioxide, and performing supercritical extraction: when the pressure of the extraction kettle I reaches 25MPa, opening a fine tuning valve F1 when the temperature of the extraction kettle I is 45 ℃, keeping the pressure and the temperature of the extraction kettle I, introducing supercritical carbon dioxide into a separation kettle I2-2, keeping the pressure of the separation kettle I at 8MPa, opening the fine tuning valve F2 when the temperature is 50 ℃, keeping the pressure and the temperature of the separation kettle I, introducing supercritical carbon dioxide into a separation kettle II 2-3, keeping the pressure of the separation kettle II at 5.5MPa, keeping the temperature at 50 ℃, and keeping the flow rate at 110-120L/h for 5h, wherein the extraction time is 5h, and the ganoderma lucidum spore oil obtained from a collection valve C1 of the separation kettle I is about 1.9kg, and has slightly turbid appearance; about 0.3kg of ganoderma lucidum spore oil is obtained from a collecting valve C2 of a separating kettle II, the appearance is turbid, the ganoderma lucidum spore oil has peculiar smell, and the ganoderma lucidum spore oil is discarded.
Mixing 300g of ganoderma lucidum spore oil obtained from the separation kettle I with 30g of ganoderma lucidum fruiting body volatile oil, standing, separating oil from water, and carrying out suction filtration on filter paper to obtain 321g of ganoderma lucidum spore oil with strong ganoderma lucidum fungus taste.
Example 2
The combined extraction-temperature-varying pressure-varying rectification equipment using supercritical carbon dioxide as shown in figure 2 is improved on the basis of the conventional supercritical extraction separation equipment, an extraction kettle II and a rectification column are added, one separation kettle is reduced, specifically, the equipment is formed by sequentially connecting an extraction kettle I1-1, an extraction kettle II 1-2, a rectification column 2-1, a separation kettle II 2-3, a heat exchanger I3-1, a storage tank 4, a high-pressure pump 5 and a heat exchanger II 3-2 through pipelines, and the heat exchanger II 3-2 is connected with the extraction kettle I to form closed loop connection. There is valve V2 on the connecting line between extraction cauldron I1-1 and the extraction cauldron II 1-2, there is valve V7 and fine setting valve F1 between the pipeline of extraction cauldron II 1-2 and rectifying column 2-1, there is fine setting valve F2 between rectifying column 2-1 and separation cauldron II 2-3, there is valve V3 between separation cauldron II 2-3 and heat exchanger I3-1, there is valve V4 between storage tank 4 and high-pressure pump 5, there is valve V5 between high-pressure pump 5 and heat exchanger II 3-2, there is valve V1 between heat exchanger II 3-2 and extraction cauldron I1-1, there is valve V6 between heat exchanger II 3-2 and extraction cauldron II, there is collection valve C1 below rectifying column 2-1, there is collection valve C2 below separation cauldron II 2-3. The rectifying column 2-1 is divided into four different temperature changing sections from bottom to top, namely a temperature changing section T1 and a temperature changing section T4.
A method for extracting Ganoderma spore oil with natural flavor by supercritical carbon dioxide combined extraction-temperature and pressure changing rectification technical equipment (figure 2) comprises the following steps: 1, 7kg of raw material I (ganoderma lucidum fruiting body particles) is taken and put into an extraction kettle I for sealing.
2, taking 7kg of raw material II (broken ganoderma lucidum spore particles), putting the raw material into an extraction kettle II, sealing, putting raw materials with high extraction rate into a general extraction kettle II, and putting raw materials with low extraction rate into an extraction kettle I.
3, opening a valve V1, a valve V2, a valve V4-valve V7, a fine tuning valve F1 and a fine tuning valve F2, wherein the rest is in a closed state, introducing carbon dioxide, boosting, simultaneously raising the temperatures of an extraction kettle I, an extraction kettle II, a rectifying column and a separation kettle II to 30 ℃, closing the fine tuning valve F2 when the pressure of the separation kettle II is 5.5MPa, and raising the temperature of the separation kettle II to 50 ℃; when the pressure of the rectifying column is 12MPa, closing a fine tuning valve F1, keeping the pressure of the rectifying column, raising the temperature of the rectifying column to (a temperature change section T1=35 ℃, a temperature change section T2=40 ℃, a temperature change section T3=45 ℃, a temperature change section T4=50 ℃), closing valves V1 and V2, raising the temperature of the extracting kettle I to 45 ℃, and carrying out static extraction on the raw material I; when the pressure of the extraction kettle II is 25MPa, the valve V3 and the fine tuning valves F1 and F2 are opened, and when the pressure of the extraction kettle II is kept, the temperature of the extraction kettle II is raised to 45 ℃, and the raw material II is dynamically extracted.
And 4, after the raw material II is dynamically extracted for 0.5h, collecting spore oil with turbid appearance, residual moisture and peculiar smell from the positions of the collecting valves C1 and C2, and discarding the spore oil. Opening valves V1 and V2, closing valve V6, raising the pressure of extraction kettle I from 12MPa to 25MPa, maintaining the pressure and temperature of extraction kettles I and II, dynamically extracting raw materials I and II simultaneously, rectifying and mixing Ganoderma spore oil and volatile oil of Ganoderma fruiting body in rectifying column, collecting Ganoderma spore oil with Ganoderma fungus taste from 1h every interval of 0.5h, adjusting fine tuning valves F1 and F2 during the process, reducing flow rate passing through extraction kettle II, reducing Ganoderma spore oil collection amount to 150g/h, and adjusting pressure of extraction kettles I and II to 20MPa by adjusting fine tuning valve F1, or reducing Ganoderma spore oil collection amount every 1h by raising the temperature of extraction kettle II to 50deg.C. The ganoderma lucidum spore oil with strong ganoderma lucidum fungus taste is collected from the valve C1, and the ganoderma lucidum spore oil is collected from the valve C2.
5, when the extraction kettle I and the extraction kettle II are used for simultaneous extraction, the fine adjustment valve F2 is adjusted, the pressure of the rectifying column is reduced by 0.5Mpa per hour, after 3 hours of extraction, the total amount of ganoderma lucidum spore oil II-1 with ganoderma lucidum fungus taste is collected from the valve C1 to about 455g, and the total amount of ganoderma lucidum spore oil II-2 is collected from the valve C2 to about 50g. Starting from 3.5h, the collected ganoderma lucidum spore oil does not have ganoderma lucidum smell any more, and the ganoderma lucidum spore oil can be continuously collected, and can be used for other purposes at the moment, or the ganoderma lucidum spore oil II with strong ganoderma lucidum smell is mixed and diluted into the ganoderma lucidum spore oil with light ganoderma lucidum smell.
After completion of the extraction, the raw material I in the extraction vessel I was taken out and weighed to obtain about 6.8kg, which indicates that about 200g of the fat-soluble components contained in the raw material I were extracted. As the late-stage ganoderma lucidum spore oil has no ganoderma lucidum smell, the ganoderma lucidum fruiting body volatile oil is completely extracted and is completely mixed with the ganoderma lucidum spore oil.
Example 3
A method for extracting Ganoderma spore oil with natural flavor by supercritical carbon dioxide combined extraction-temperature and pressure changing rectification technical equipment (figure 2) comprises the following steps: 1, 7kg of raw material II is taken and put into an extraction kettle II, and the extraction kettle II is sealed.
2, collecting radix Panacis Quinquefolii (raw material III) (dried root of Panax quinquefolium of Araliaceae Panax quinquefolium L), sieving to remove impurities, oven drying at 50deg.C until water content is below 3%, pulverizing into granule, taking 10kg as raw material III, adding into extraction kettle I, and sealing.
3, opening a valve V1, a valve V2, a valve V4-valve V7, a fine tuning valve F1 and a fine tuning valve F2, wherein the rest is in a closed state, introducing carbon dioxide, boosting, and simultaneously raising the temperatures of an extraction kettle I, an extraction kettle II, a rectifying column and a separation kettle II to 30 ℃, when the pressure of the separation kettle II is 5.5MPa, closing the fine tuning valve F2, and raising the temperature of the separation kettle II to 50 ℃; when the pressure of the rectifying column is 10MPa, closing a fine tuning valve F1, keeping the pressure of the rectifying column, raising the temperature of the rectifying column to (a temperature change section T1=35 ℃, a temperature change section T2=40 ℃, a temperature change section T3=45 ℃, a temperature change section T4=50 ℃), closing valves V1 and V2, raising the temperature of an extraction kettle I to 50 ℃, and carrying out static extraction on a raw material III; when the pressure of the extraction kettle II is 25MPa, the valve V3 is opened, the valves F1 and F2 are finely adjusted, and when the pressure of the extraction kettle II is kept, the temperature of the extraction kettle II is raised to 45 ℃, and the raw material II is dynamically extracted.
And 4, after the raw material II is dynamically extracted for 0.5h, collecting spore oil with turbid appearance, residual moisture and peculiar smell from the positions of the valves C1 and C2, and discarding the spore oil. Opening valves V1 and V2, closing valve V6, raising the pressure of extraction kettle I from 10MPa to 25MPa, maintaining the pressure and temperature of extraction kettles I and II, dynamically extracting raw materials III and II simultaneously, rectifying and mixing ganoderma lucidum spore oil and American ginseng volatile oil in a rectifying column, collecting ganoderma lucidum spore oil with American ginseng taste from 1h every 0.5h, adjusting fine tuning valves F1 and F2 during the process, increasing the flow rate passing through extraction kettle II, raising the collection amount of ganoderma lucidum spore oil to 300g/h, and also adjusting the pressure of extraction kettles I and II to 30MPa by adjusting fine tuning valve F1, or reducing the temperature of extraction kettle II to 40 ℃ to improve the collection amount of ganoderma lucidum spore oil every 1 h. Ganoderma spore oil having strong American ginseng flavor was collected from valve C1. Ganoderma spore oil with light American ginseng taste was collected from valve C2.
And 5, when the extraction kettle I and the extraction kettle II are used for simultaneous extraction, the pressure of the rectifying column is reduced by 0.5Mpa per hour by adjusting the fine adjustment valve F2, and after 3 hours of extraction, the ganoderma lucidum spore oil III-1 with American ginseng taste is collected from the valve C1 for a total of about 910g. The ganoderma lucidum spore oil III-2 with American ginseng taste is collected from the valve C2 for about 85g in total, and the collected ganoderma lucidum spore oil no longer has American ginseng taste from 3.5 hours, which means that the American ginseng volatile oil is completely extracted and completely mixed with the ganoderma lucidum spore oil. The Ganoderma spore oil can be continuously collected, and can be used for other purposes, or diluted into Ganoderma spore oil with light American ginseng taste by mixing with Ganoderma spore oil with strong American ginseng taste.
Example 4
A method for extracting Ganoderma spore oil with natural flavor by supercritical carbon dioxide combined extraction-temperature and pressure changing rectification technical equipment (figure 2) comprises the following steps: 1, taking 7kg of a raw material II, putting the raw material II into an extraction kettle II of supercritical carbon dioxide combined extraction-variable temperature and pressure rectification technical equipment, and sealing.
2, taking jasmine flower (raw material IV) (flowers of Jasminum sambac (L.) Aiton of Oleaceae), sieving to remove impurities, drying at 50deg.C until the water content is below 3%, recording as raw material IV, taking 3kg, adding into an extraction kettle I of supercritical carbon dioxide combined extraction-variable temperature and pressure rectification technical equipment, and sealing.
3, opening a valve V1, a valve V2, a valve V4-valve V7, a fine tuning valve F1 and a fine tuning valve F2, and closing the rest, introducing carbon dioxide, boosting, and simultaneously raising the temperatures of an extraction kettle I, an extraction kettle II, a rectifying column and a separation kettle II to 30 ℃, when the pressure of the separation kettle II is 5.5MPa, closing the fine tuning valve F2, and raising the temperature of the separation kettle II to 50 ℃; when the pressure of the rectifying column is 12MPa, closing a fine tuning valve F1, keeping the pressure of the rectifying column, raising the temperature of the rectifying column to (a temperature change section T1=35 ℃, a temperature change section T2=40 ℃, a temperature change section T3=45 ℃, a temperature change section T4=50 ℃), closing valves V1 and V2, raising the temperature of an extraction kettle I to 40 ℃, and carrying out static extraction on a raw material IV; when the pressure of the extraction kettle II is 25MPa, the valve V3 is opened, the valves F1 and F2 are finely adjusted, and when the pressure of the extraction kettle II is kept, the temperature of the extraction kettle II is raised to 45 ℃, and the raw material II is dynamically extracted.
And 4, after the raw material II is dynamically extracted for 0.5h, collecting spore oil with turbid appearance, residual moisture and peculiar smell from the positions of the valves C1 and C2, and discarding the spore oil. Opening valves V1 and V2, closing valve V6, raising the pressure of extraction kettle I from 12MPa to 25MPa, maintaining the pressure and temperature of extraction kettles I and II, dynamically extracting raw materials IV and II simultaneously, rectifying and mixing Ganoderma spore oil and volatile oil of jasmine flower in a rectifying column, collecting Ganoderma spore oil with jasmine flower taste from 0.5h every interval, adjusting fine tuning valves F1 and F2 during the process, reducing the flow rate passing through extraction kettle II, reducing the collection amount of Ganoderma spore oil to 100g/h, and adjusting the pressure of extraction kettles I and II to 20MPa or raising the temperature of extraction kettle II to 50 ℃ by adjusting fine tuning valve F1, and reducing the collection amount of Ganoderma spore oil every 1 h. The ganoderma lucidum spore oil with strong jasmine flower taste is collected from the valve C1, and the ganoderma lucidum spore oil with light jasmine flower taste is collected from the valve C1.
And 5, when the extraction kettle I and the extraction kettle II are used for simultaneous extraction, the pressure of the rectifying column is reduced by 0.5Mpa per hour by adjusting the fine adjustment valve F2, and after 2 hours of extraction, the ganoderma lucidum spore oil IV-1 with jasmine flower taste is collected from the valve C1 for a total of about 205g. The total of about 75g of ganoderma lucidum spore oil IV-2 with jasmine flower taste is collected from the valve C2, and the collected ganoderma lucidum spore oil does not have jasmine flower taste from 2.5 hours, which means that the jasmine flower volatile oil is completely extracted and completely mixed with the ganoderma lucidum spore oil. The ganoderma lucidum spore oil can be continuously collected from the valve C1, and can be used for other purposes at the moment, or the ganoderma lucidum spore oil with strong jasmine flower taste is mixed and diluted into the ganoderma lucidum spore oil with light jasmine flower taste.
Experimental test example
The ganoderma lucidum spore oils I, II-1, III-1, IV-1, II-2, III-2, IV-2 were sampled to detect acid value, peroxide value, clarity and sense, the results are shown in Table 1,
ganoderma spore oil I, II-1, III-1, IV-1 is sealed in oral liquid bottle, sealed, placed at 37deg.C and 75% humidity, and tested for acid value, peroxide value, clarity and sense every 2 months for stability investigation, and the results are shown in tables 2-5.
The method for detecting the acid value is GB 5009.229 method for detecting the peroxide value in food safety national standard food, the method for detecting the peroxide value in GB 5009.227 food safety national standard food, the method for detecting the clarity of the food is national pharmacopoeia four general rules 0902 method for detecting the sense organ of the food safety national standard vegetable oil, and the method for evaluating the sense organ of the food safety national standard vegetable oil is GB2716
Table 1 test results at 0 th month
The acid values and peroxide values of the I, II-2, III-2 and IV-2 are close to or exceed the GB2716 standard, and the compound is not suitable to be used as a food raw material. The subsequent detection of II-2, III-2 and IV-2 is not continued, but I is used as a comparison sample to participate in the subsequent detection.
Table 2 month 2 test results
Table 3 4 th month test results
Table 4 results of 6 th month test
Table 5 results of 8 th month test
As can be seen from tables 1-5, the acid value and peroxide value of ganoderma lucidum spore oil I in the stability test result of month 2 are close to or exceed the GB2716 standard, and are not suitable as food raw materials. But the fragrance can be stably maintained until month 8;
the acid value and peroxide value of the ganoderma lucidum spore oil II-1 are always smaller than the GB2716 standard, and the fragrance can be stably maintained to 8 months, so that the ganoderma lucidum spore oil is suitable to be used as a raw material of food, health-care food or cosmetics;
the acid value and peroxide value of the ganoderma lucidum spore oil III-1 are always smaller than the GB2716 standard, and the fragrance can be stably kept to 8 months, but the effect is inferior to II-1, so that the ganoderma lucidum spore oil is suitable for being used as a raw material of food, health-care food or cosmetics;
the acid value and peroxide value of the ganoderma lucidum spore oil IV-1 are always smaller than the GB2716 standard, but the fragrance can be stably maintained until the month 6, and the ganoderma lucidum spore oil is also suitable to be used as a raw material of food, health-care food or cosmetics;
the technical effect of mixing natural product volatile oil with Ganoderma spore oil as carrier is best achieved by supercritical carbon dioxide combined extraction-variable temperature and pressure rectification technique. The acid value, the peroxide value and the like of the ganoderma lucidum spore oil are superior to those of the ganoderma lucidum spore oil obtained by mixing the volatile oil of the natural product after supercritical extraction. Meanwhile, the flavor components of the ganoderma lucidum spore oil can exist stably for more than or equal to 6 months under the condition that the ambient temperature is less than or equal to 37 ℃.
Claims (4)
1. A ganoderma lucidum spore oil with natural flavor is characterized in that: extracting fat-soluble components in ganoderma lucidum spore powder and fat-soluble components of other natural products by adopting a supercritical carbon dioxide combined extraction technology, and obtaining the ganoderma lucidum spore powder by fully mixing volatile oil of other natural products by taking ganoderma lucidum spore oil as a carrier in the separation process and removing impurities; the supercritical carbon dioxide combined extraction technology refers to: during supercritical extraction, extracting Ganoderma spore powder and other natural products in different extraction kettles, and conveying liposoluble components of Ganoderma spore powder and liposoluble components of other natural products dissolved in supercritical carbon dioxide into a rectifying column; the extraction process of the fat-soluble components of the ganoderma lucidum spore powder and the fat-soluble components of other natural products comprises the following steps: collecting mature ganoderma spores, collecting into powder, sieving to remove impurities, breaking wall, granulating, oven drying until the water content is below 3%, taking wall-broken ganoderma spore powder particles with a certain weight, putting into an extraction kettle II of a supercritical extraction device, sealing, introducing carbon dioxide, boosting a separation kettle-rectifying column-extraction kettle II-extraction kettle I in sequence, and performing supercritical extraction after the rectifying column reaches a set pressure and temperature: the pressure of the extraction kettle II is 20-25 MPa, and the extraction temperature is 40-50 ℃; collecting other natural products, sieving to remove impurities, grinding, granulating, oven drying until the water content is below 3%, taking other natural products with certain weight, putting into an extraction kettle I of a supercritical extraction device, sealing, introducing supercritical carbon dioxide, and performing supercritical extraction: the pressure of the extraction kettle I is 20-25 MPa, the extraction temperature is 40-50 ℃, the combined extraction of the wall-broken ganoderma lucidum spore powder and other natural products is carried out simultaneously or at intervals, the extraction kettle II and the extraction kettle I can extract fat-soluble components with different specifications from the wall-broken ganoderma lucidum spore powder and other natural products under different pressures and temperatures, the flow rate during the extraction is 110-120L/h, and the extraction time is 2-3 h; the separation process of volatile oil components in ganoderma lucidum spore oil and other natural products comprises the following steps: when the combined extraction of the wall-broken ganoderma lucidum spore powder and other natural products is started, the extraction pressure of a rectifying column is 8-12 MPa, the rectifying column is divided into a plurality of variable temperature sections, the temperature of each section is 35-50 ℃, the length of the rectifying column is that the diameter=30:1, the rectifying column is filled with filler, the filler is made of stainless steel or ceramic, and ganoderma lucidum spore oil with different flavors is collected from the rectifying column under different pressures and temperatures.
2. The ganoderma lucidum spore oil with natural flavor according to claim 1, wherein the temperature-variable pressure-variable rectification technology is that the ganoderma lucidum spore oil and volatile oil of carbon dioxide dissolved in a supercritical state are separated out due to the reduced solubility caused by the pressure change under the temperature and pressure regulation of a rectification column; purifying by temperature difference change of temperature change section of rectifying column, mixing volatile oil with Ganoderma spore oil as carrier, and removing impurities.
3. The ganoderma lucidum spore oil with natural flavor according to claim 1, wherein the rectifying column is divided into four sections, the temperature varying section t1=35 ℃, the temperature varying section t2=40 ℃, the temperature varying section t3=45 ℃, and the temperature varying section t4=50 ℃.
4. The ganoderma lucidum spore oil with natural flavor according to claim 1, wherein the flavor component of the ganoderma lucidum spore oil with natural flavor can exist stably for more than or equal to 6 months at the ambient temperature of less than or equal to 37 ℃.
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