CN112680275A - Supercritical extraction process of ganoderma lucidum spore oil with high extraction rate - Google Patents
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- 240000008397 Ganoderma lucidum Species 0.000 title claims abstract description 62
- 235000001637 Ganoderma lucidum Nutrition 0.000 title claims abstract description 62
- 238000000605 extraction Methods 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000000194 supercritical-fluid extraction Methods 0.000 title claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 48
- 238000004880 explosion Methods 0.000 claims abstract description 48
- 238000000926 separation method Methods 0.000 claims abstract description 44
- 241000222336 Ganoderma Species 0.000 claims abstract description 35
- 239000000843 powder Substances 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002002 slurry Substances 0.000 claims abstract description 14
- 238000011282 treatment Methods 0.000 claims abstract description 8
- 238000007791 dehumidification Methods 0.000 claims abstract description 7
- 238000011278 co-treatment Methods 0.000 claims abstract description 3
- 238000010257 thawing Methods 0.000 claims description 9
- 230000008014 freezing Effects 0.000 claims description 8
- 238000007710 freezing Methods 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 6
- 238000005469 granulation Methods 0.000 claims description 6
- 230000003179 granulation Effects 0.000 claims description 6
- 229940031703 low substituted hydroxypropyl cellulose Drugs 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- 239000008187 granular material Substances 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 150000003648 triterpenes Chemical class 0.000 abstract description 10
- 235000019441 ethanol Nutrition 0.000 description 13
- 230000000694 effects Effects 0.000 description 7
- 238000005422 blasting Methods 0.000 description 6
- 238000011068 loading method Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000007908 dry granulation Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000006837 decompression Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003359 percent control normalization Methods 0.000 description 2
- 238000011112 process operation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000004671 saturated fatty acids Chemical class 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
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Abstract
The invention relates to a supercritical extraction process of ganoderma lucidum spore oil with high extraction rate, belonging to the technical field of ganoderma lucidum spore oil extraction. A supercritical extraction process of Ganoderma spore oil with high extraction rate comprises the following steps: step 1) freeze-thaw operation: taking fresh ganoderma lucidum spore powder for freeze-thaw cycle treatment; step 2) steam explosion: performing steam explosion on the frozen and thawed ganoderma lucidum spore powder, and performing explosion by using ethanol steam and water steam as explosion media to obtain ganoderma lucidum spore slurry; step 3) granulating: carrying out reduced pressure dehumidification on the obtained ganoderma lucidum spore slurry and then granulating; step 4), supercritical extraction: subjecting Ganoderma spore powder to supercritical CO treatment2Extracting; step 5) separation: separating the extract by three-stage reduced pressure separation, and collecting the ganoderma lucidum spore oil in the separation kettle I and the separation kettle II. The method has the advantages of high extraction rate of the ganoderma lucidum spore oil and high content of total triterpenes of effective components.
Description
Technical Field
The invention belongs to the technical field of ganoderma lucidum spore oil extraction, and particularly relates to a high-extraction-rate ganoderma lucidum spore oil supercritical extraction process.
Background
The ganoderma spore oil is an oily lipid substance extracted from wall-broken ganoderma spores by an extraction technology, mainly contains saturated fatty acid and unsaturated fatty acid and various active ingredients of the ganoderma spores, and is a yellow transparent liquid. Modern researches prove that the ganoderma lucidum spore oil has the functions of improving immunity, resisting oxidation of organisms and the like, and has a better health-care effect.
Supercritical CO2The extraction technology is the mainstream technology for extracting ganoderma spore oil from ganoderma spore powder at present, and CN102011163B discloses a multi-body multi-stage supercritical CO2A method for extracting ganoderma spore oil comprises granulating superfine pulverized wall-broken ganoderma spore powder, and separating by supercritical CO with three-stage separation2The method can realize the separation of the ganoderma lucidum spore oil and the entrainer in the extraction process, and has the defects that the wall breaking rate of the ganoderma lucidum spore powder is lower due to superfine grinding wall breaking, so that the extraction rate of the ganoderma lucidum spore oil is lower.
Disclosure of Invention
Based on the problem of low extraction rate of the ganoderma spore powder spore oil in the prior art, the invention aims to provide the ganoderma spore oil supercritical extraction process with high extraction rate, and the extraction rate of the ganoderma spore oil can be effectively improved by the process.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
the invention provides a supercritical extraction process of ganoderma lucidum spore oil with high extraction rate, which comprises the following steps:
step 1) freeze-thaw operation: taking fresh ganoderma lucidum spore powder for freeze-thaw cycle treatment;
step 2) steam explosion: and (3) performing steam explosion on the freeze-thawed ganoderma lucidum spore powder, introducing ethanol steam until the pressure in an explosion container is 0.8-1.2 MPa, introducing water steam until the pressure in the explosion container is 1.5-1.8 MPa, and maintaining the pressure for 50-60 s to obtain ganoderma lucidum spore slurry.
Step 3) granulating: carrying out reduced pressure dehumidification on the obtained ganoderma lucidum spore slurry and then granulating;
step 4), supercritical extraction: subjecting Ganoderma spore powder to supercritical CO treatment2Extracting;
step 5) separation: separating the extract by three-stage reduced pressure separation, and collecting the ganoderma lucidum spore oil in the separation kettle I and the separation kettle II.
In the method, the surface of the ganoderma lucidum spore powder is cracked through repeated freeze thawing operation, so that the permeation of ethanol steam is facilitated, and the blasting effect of the blasting medium on the ganoderma lucidum spore powder is improved. The aim of dehumidifying the ganoderma spore slurry obtained after steam explosion by adopting a decompression technology is to reduce the moisture content of the ganoderma spore slurry by decompressing and dehumidifying, thereby being beneficial to the smooth proceeding of the subsequent dry granulation process.
Further, repeated freezing and thawing operation is beneficial to generating tiny cracks on the surface of the ganoderma lucidum spore powder through temperature change, tests show that the freezing and thawing cycle in the step 1) is that the spore powder is frozen for 12-16 h at-15 to-18 ℃ and thawed for 6-8 h at 20-25 ℃, the cycle frequency is 5-10 times, and the freezing and thawing operation and steam explosion under the conditions can achieve a good explosion effect.
Further, the separation pressure of the separation kettle I in the step 5) is 12-14 MPa, and the temperature is 40-45 ℃.
Further, the separation pressure of the separation kettle II in the step 5) is 8-9 MPa, and the temperature is 35-45 ℃.
In a specific embodiment, the separation pressure of the separation kettle I adopted by the invention is 13MPa, the temperature is 42 ℃, the separation pressure of the separation kettle II is 8.5MPa, the temperature is 40 ℃, and the separation pressure of the separation kettle III is 5.5 MPa.
Further, the decompression dehumidification in the step 3) is carried out in low-temperature vacuum drying equipment, and the temperature is 40-50 ℃.
Further, in the step 3), the moisture content of the blasted ganoderma lucidum spore material after dehumidification is 20-30%.
Further, the granulation in the step 3) also comprises the step of mixing the dehumidified blasting ganoderma lucidum spore with low-substituted hydroxypropyl cellulose with the mass of 5-10%. The low-substituted hydroxypropyl cellulose has a good bonding effect on the blasting ganoderma lucidum spore substances and cannot generate any reaction with the ganoderma lucidum spore oil, the particles obtained by mixing and granulating the low-substituted hydroxypropyl cellulose serving as an adhesive with the blasting ganoderma lucidum spore substances have good particle uniformity, the spore powder is not easy to be taken away by an extracting agent in the supercritical extraction process to cause the blockage of extraction equipment by adopting dry granulation, and the structure of the particles has certain looseness to be beneficial to the extraction of the spore oil in the spore powder.
Further, the mesh number of the granulation in the step 3) is 40-50 meshes, and the dry granulation is adopted in the granulation process.
Further, the ethanol vapor is saturated vapor of anhydrous ethanol.
Further, the specific conditions of the supercritical extraction in the step 4) are as follows: the extraction pressure is 20-30 MPa, the extraction temperature is 40-50 ℃, the extraction time is 30-60 min, and the flow rate of carbon dioxide is 20-50L/h.
The supercritical extraction process of the ganoderma lucidum spore oil with high extraction rate provided by the preferred embodiment of the invention has the beneficial effects that: by adopting the extraction method, the freeze-thawing operation, the double-solvent steam explosion treatment, the granulation and the supercritical extraction operation are sequentially adopted, and specific process operation parameters are combined, so that the synergistic effect can be realized from the whole, the higher extraction rate of the ganoderma lucidum spore oil is finally obtained, and the total triterpene content of the effective components in the ganoderma lucidum spore oil is higher.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
Taking 10kg of fresh ganoderma lucidum spore powder, hermetically packaging, placing in a refrigerator, freezing at-18 ℃ for 12h, taking out, and melting at 25 ℃ for 6h, wherein the cycle time is 8 times; loading freeze-thawed Ganoderma spore powder into steam explosion chamber, introducing ethanol steam until the pressure in the explosion container is 1.0MPa, and thenIntroducing water vapor until the pressure in the explosion container is 1.5MPa, maintaining the pressure for 50s, instantaneously exploding to obtain Ganoderma spore slurry containing water and ethanol, vacuum drying at 45 deg.C under reduced pressure to obtain exploded Ganoderma spore with moisture content of 26.3%, adding 8% of low-substituted hydroxypropyl cellulose into the exploded Ganoderma spore, mixing, dry pressing into 40-mesh granules, and transferring into supercritical CO2In the extraction kettle, the selected extraction pressure is 25MPa, the extraction temperature is 45 ℃, the extraction time is 45min, and the flow rate of carbon dioxide is 30L/h. The separation pressure of the separation kettle I is 13MPa, the temperature is 42 ℃, the separation pressure of the separation kettle II is 8.5MPa, the temperature is 40 ℃, the separation pressure of the separation kettle III is 5.5MPa, and the temperature is 38 ℃; and finally, 3.12kg of the ganoderma lucidum spore oil component with weak polarity is discharged from the separation kettle I, and the oil yield is 31.2%. 0.69kg of highly polar ganoderma lucidum spore oil discharged from the separation kettle II, the oil yield is 6.9%, wherein the total triterpene content is 20.1%.
Examples 2 to 4
Extracting ganoderma lucidum spore oil according to the raw materials and the process in the embodiment 1, and performing tests on the influence of different times of freeze-thaw cycles on the oil yield of ganoderma lucidum spore oil, wherein the difference is that the freeze-thaw cycles selected in the embodiment 2 are 1, the freeze-thaw cycles selected in the embodiment 3 are 3, the freeze-thaw cycles selected in the embodiment 4 are 5, and meanwhile, blank controls are set, and no freeze-thaw operation is performed during steam explosion of ganoderma lucidum spore powder, and the test results are shown in table 1:
table 1: effect of different number of freeze-thaw cycles on extraction Rate
| Numbering | Oil yield of separation kettle I | Oil yield of separation kettle II | Separation vessel II Total triterpene content |
| Example 2 | 20.8% | 4.6% | 20.8% |
| Example 3 | 22.5% | 3.7% | 19.8% |
| Example 4 | 30.8% | 6.4% | 21.4% |
| Blank control | 18.5% | 3.5% | 19.2% |
Comparing the process conditions of the examples 1-4 and the blank control with the extraction yield of the ganoderma lucidum spore oil and the like, it can be known that the freeze-thaw operation of the ganoderma lucidum spore powder before steam explosion has significant influence on the extraction rate of the ganoderma lucidum spore oil, but has little influence on the content of the total triterpenoids; wherein, single freezing and thawing operation and no freezing and thawing operation treatment are carried out, the difference value of the extraction rate results of the ganoderma lucidum spore oil is not large, and the oil yield of the ganoderma lucidum spore oil in the separation kettle I and the separation kettle II can be obviously improved only by 5 times or more of freezing and thawing cycle operation combined with steam explosion.
Examples 5 to 7
Extracting the ganoderma lucidum spore oil according to the raw materials and the process in the embodiment 1, and carrying out different steam explosion treatments to influence the oil yield of the ganoderma lucidum spore oil, wherein the difference is as follows:
example 5 specific conditions for steam explosion selected: loading freeze-thawed Ganoderma spore powder into steam explosion cavity, introducing ethanol steam until the pressure in the explosion container is 0.8MPa, introducing water steam until the pressure in the explosion container is 1.5MPa, maintaining the pressure for 50s, instantaneously exploding to obtain Ganoderma spore slurry containing water and ethanol, and vacuum drying at 45 deg.C under reduced pressure to obtain exploded Ganoderma spore with moisture content of 28.7%.
Example 6 specific conditions for steam explosion selected: loading freeze-thawed Ganoderma spore powder into steam explosion cavity, introducing ethanol steam until the pressure in the explosion container is 1.2MPa, introducing water steam until the pressure in the explosion container is 1.5MPa, maintaining the pressure for 50s, instantaneously exploding to obtain Ganoderma spore slurry containing water and ethanol, and vacuum drying at 45 deg.C under reduced pressure to obtain exploded Ganoderma spore with moisture content of 26.9%.
Example 7 specific conditions for steam explosion selected: loading freeze-thawed Ganoderma spore powder into steam explosion cavity, introducing ethanol steam until the pressure in the explosion container is 1.2MPa, introducing water steam until the pressure in the explosion container is 1.8MPa, maintaining the pressure for 50s, instantaneously exploding to obtain Ganoderma spore slurry containing water and ethanol, and vacuum drying at 45 deg.C under reduced pressure to obtain exploded Ganoderma spore with moisture content of 26.9%.
Specific conditions for steam explosion selected in control 1: loading freeze-thawed Ganoderma spore powder into steam explosion chamber, introducing steam until the pressure in the explosion container is 1.8MPa, maintaining the pressure for 50s, performing instantaneous explosion to obtain Ganoderma spore slurry containing water, and vacuum drying at 55 deg.C under reduced pressure to obtain blasted Ganoderma spore with moisture content of 28.5%.
Specific conditions for steam explosion selected in control 2: loading freeze-thawed Ganoderma spore powder into steam explosion chamber, introducing steam until the pressure in the explosion container is 1.8MPa, maintaining the pressure for 50s, performing instantaneous explosion to obtain Ganoderma spore slurry containing water, and vacuum drying at 45 deg.C under reduced pressure to obtain blasted Ganoderma spore with moisture content of 26.9%.
Wherein, in comparison 2, 340g of absolute ethyl alcohol is added as entrainer in the supercritical extraction process according to the content of ethyl alcohol in the ganoderma lucidum spore powder particles in the embodiment 1.
The test results of examples 5 to 7 and controls 1 to 2 are shown in Table 2:
table 2: effect of different steam explosion on extraction yield
| Numbering | Oil yield of separation kettle I | Oil yield of separation kettle II | Separation vessel II Total triterpene content |
| Example 5 | 30.7% | 7.1% | 20.5% |
| Example 6 | 30.5% | 7.2% | 19.4% |
| Example 7 | 29.6% | 7.4% | 21.2% |
| Control 1 | 24.8% | 6.9% | 18.3% |
| Control 2 | 25.1% | 5.6% | 18.5% |
Comparing the process conditions of examples 5 to 7 with those of example 1 and the extraction yield of the ganoderma lucidum spore oil, it can be seen that the oil yield and quality of the ganoderma lucidum spore oil obtained by performing steam explosion on the freeze-thawed ganoderma lucidum spore powder by using the process conditions of examples 5 to 7 can achieve the effects of example 1. As can be seen from comparison of the results of examples 5-7 with those of controls 1-2, the extraction rate and the total triterpene content of the ganoderma lucidum spore oil are both significantly reduced by using water vapor alone as the blasting medium, and even if a certain amount of ethanol is supplemented as the entrainer in the supercritical extraction process, the extraction rate and the total triterpene content in control 2 are not significantly improved on the basis of control 1. It is shown that the influence of the ethanol steam and the water steam on the extraction rate and the total triterpene content of the ganoderma lucidum spore oil in the steam explosion stage can not be only attributed to the fact that the double-solvent steam explosion treatment influences the content of the solvent in the ganoderma lucidum spore particles in the subsequent supercritical extraction process, so that the extraction method provided by the invention sequentially adopts the freeze-thaw operation, the double-solvent steam explosion treatment, the granulation and the supercritical extraction operation, and combines specific process operation parameters, and the synergistic effect can be achieved from the whole body, and finally the higher extraction rate of the ganoderma lucidum spore oil and the higher total triterpene content can be obtained.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (10)
1. A supercritical extraction process of ganoderma lucidum spore oil with high extraction rate is characterized by comprising the following steps:
step 1) freeze-thaw operation: taking fresh ganoderma lucidum spore powder for freeze-thaw cycle treatment;
step 2) steam explosion: performing steam explosion on the freeze-thawed ganoderma lucidum spore powder, introducing ethanol steam until the pressure in an explosion container is 0.8-1.2 MPa, introducing water steam until the pressure in the explosion container is 1.5-1.8 MPa, and maintaining the pressure for 50-60 s to obtain ganoderma lucidum spore slurry;
step 3) granulating: carrying out reduced pressure dehumidification on the obtained ganoderma lucidum spore slurry and then granulating;
step 4), supercritical extraction: subjecting Ganoderma spore powder to supercritical CO treatment2Extracting;
step 5) separation: separating the extract by three-stage reduced pressure separation, and collecting the ganoderma lucidum spore oil in the separation kettle I and the separation kettle II.
2. The extraction process according to claim 1, wherein the freeze-thaw cycle in the step 1) is freezing the spore powder at-15 to-18 ℃ for 12 to 16 hours and thawing the spore powder at 20 to 25 ℃ for 6 to 8 hours, and the number of cycles is 5 to 10.
3. The extraction process according to claim 1, wherein the separation pressure of the separation kettle I in the step 5) is 12-14 MPa, and the temperature is 40-45 ℃.
4. The extraction process according to claim 1, wherein the separation pressure of the separation kettle II in the step 5) is 8-9 MPa, and the temperature is 35-45 ℃.
5. The extraction process according to claim 1, wherein the reduced pressure dehumidification in step 3) is performed in a low temperature vacuum drying device, and the temperature is 40-50 ℃.
6. The extraction process according to claim 1, wherein the moisture content of the blasted ganoderma lucidum spores after dehumidification in step 3) is 20-30%.
7. The extraction process according to claim 1 or 6, wherein the granulation in step 3) further comprises mixing the dehumidified ganoderma lucidum spore with 5-10% by mass of low-substituted hydroxypropylcellulose.
8. The extraction process according to claim 1, wherein the mesh size of the granules in step 3) is 40-50 mesh.
9. The extraction process according to claim 1, wherein the ethanol vapour is saturated vapour of anhydrous ethanol.
10. The extraction process according to claim 1, wherein the specific conditions of the supercritical extraction in step 4) are: the extraction pressure is 20-30 MPa, the extraction temperature is 40-50 ℃, the extraction time is 30-60 min, and the flow rate of carbon dioxide is 20-50L/h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115011407A (en) * | 2022-06-24 | 2022-09-06 | 广东钰禾生物科技有限公司 | Method for supercritical extraction of ganoderma lucidum spore oil and application of ganoderma lucidum spore oil |
| CN115216361A (en) * | 2022-08-12 | 2022-10-21 | 武夷山元生泰生物科技有限公司 | Preparation method of ganoderma lucidum spore oil |
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