CN1099455C - Process for extracting lipid matter of ganoderma spore by immersing extraction - Google Patents
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- CN1099455C CN1099455C CN00130884A CN00130884A CN1099455C CN 1099455 C CN1099455 C CN 1099455C CN 00130884 A CN00130884 A CN 00130884A CN 00130884 A CN00130884 A CN 00130884A CN 1099455 C CN1099455 C CN 1099455C
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- ganoderma spore
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- 241000222336 Ganoderma Species 0.000 title claims abstract description 137
- 150000002632 lipids Chemical class 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000000605 extraction Methods 0.000 title claims description 60
- 238000002386 leaching Methods 0.000 claims abstract description 26
- 239000011259 mixed solution Substances 0.000 claims abstract description 17
- 239000003960 organic solvent Substances 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 108010059892 Cellulase Proteins 0.000 claims abstract description 5
- 102000012286 Chitinases Human genes 0.000 claims abstract description 5
- 108010022172 Chitinases Proteins 0.000 claims abstract description 5
- 229940106157 cellulase Drugs 0.000 claims abstract description 5
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical group CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 claims description 5
- 238000011282 treatment Methods 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 3
- 238000002203 pretreatment Methods 0.000 claims 2
- 238000002791 soaking Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 14
- 239000000284 extract Substances 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract description 2
- 230000035784 germination Effects 0.000 abstract 1
- 230000003647 oxidation Effects 0.000 description 10
- 238000007254 oxidation reaction Methods 0.000 description 10
- 239000003205 fragrance Substances 0.000 description 9
- 238000001556 precipitation Methods 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 239000002775 capsule Substances 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 5
- 238000000703 high-speed centrifugation Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 210000002421 cell wall Anatomy 0.000 description 3
- 230000007071 enzymatic hydrolysis Effects 0.000 description 3
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 description 3
- 239000004519 grease Substances 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 108090000790 Enzymes Proteins 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 240000008397 Ganoderma lucidum Species 0.000 description 2
- 235000001637 Ganoderma lucidum Nutrition 0.000 description 2
- 229940088598 enzyme Drugs 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000000108 ultra-filtration Methods 0.000 description 2
- 241000233866 Fungi Species 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000002101 lytic effect Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 238000009333 weeding Methods 0.000 description 1
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Abstract
The present invention relates to a method for extracting intracapsular lipid substances of ganoderma spores by a leaching method. Ganoderma spores are soaked in organic solvents by a solid-liquid extracting principle to cause the lipid substances of the ganoderma spores to be dissolved in the solvents to form mixed solution, and the mixed solution is in air stripping to efficiently extract intracapsular lipid substances of the ganoderma spores. Ganoderma spores can be soaked to promote the ganoderma spores to be in the accelerating germination period before the ganoderma spores are extracted and leached, and be in ultramicro wall breaking by physical crushing methods, such as mechanical ultramicro crushing, etc., and chitinase and cellulase can be added into the ganoderma spores before the ganoderma spores are extracted and leached to cause the spore walls of the ganoderma spores to be softened by enzymolysis and to lose toughness. Ganoderma spore lipid substances extracted by the present invention in a lipid state account for 6% to 37% of the total weight of the ganoderma spores which are not extracted and leached.
Description
The present invention relates to a kind of method that adopts lixiviation process extracting ganoderma conidial cell wall capsule inner lipid material.
Glossy ganoderma is a Basidiomycetes polyporaceae Ganoderma fungi.Ganoderma spore is the atomic thin avette spore of brown (6-7 * 10-12 μ m) that glossy ganoderma ejects from the cap bottom vegetative period.Discover that Ganoderma spore has the whole hereditary active substance of glossy ganoderma.Because Ganoderma spore sporoderm compact structure and tough and tensile unusually, conventional extracting method are difficult to extracting to the abundant lipid matter of Ganoderma spore wall capsule intensive amount, cause having being of pharmaceutical use of crucial importance sebaceous lipid matter of ganoderma spore and be not fully utilized.
The purpose of this invention is to provide a kind of method that adopts lixiviation process extracting ganoderma conidial cell wall capsule inner lipid material, so that the pharmaceutical use of Ganoderma spore obtains more abundant application widely.
The present invention finds, adopts the organic solvent lixiviation process the sebaceous lipid matter that is that is stored in the Ganoderma spore wall capsule efficiently can be extracted, and every 100kg Ganoderma spore can extract 6～37kg lipid matter of ganoderma spore.
Method of the present invention is to adopt admittedly---the principle of liquid extraction, Ganoderma spore is dipped in the greasy organic solvent of industrial leaching commonly used, lipid matter of ganoderma spore is dissolved in forms mixed solution in the solvent, again mixed solution is carried out stripping, can make solvent vaporization and separate, thereby obtain lipid matter of ganoderma spore with lipid matter of ganoderma spore.The lipid matter of ganoderma spore of this lixiviation process extraction has original physiologically active of reservation, not oxidation, characteristics such as free from extraneous odour.
The inventive method concrete steps are as follows:
One, raw material: gather Ganoderma spore and, preferably select the Ganoderma spore of mature and plump for use through further screening.Ganoderma spore can impel Ganoderma spore to be in through immersion to sprout the vernalization phase that (water temperature of immersion is 16～49 ℃ earlier, be generally 18～42 ℃, soak time is 10min～24h, the vernalization phase humidity of sprouting is 80～100%, be generally 98%, temperature is 16～49 ℃, is generally 18～42 ℃, and the time is 10min～24h); Also can be heated to 90～120 ℃ through curing earlier, be generally 100 ℃ of thermal treatments; Also can handle through the broken wall operation earlier, to improve the lipid matter of ganoderma spore extraction yield.The broken wall operation adopts common industrial machinery micronizing, or rolls, or the physics breaking method such as grinds and make breaking trachytectum of glossy ganoderma.Can also in Ganoderma spore, add lytic enzymes such as biotechnology chitinase commonly used, cellulase before leaching extraction or before the broken wall, enzyme add-on (by weight) is 0.002～2%, be generally 0.01～0.03%, keep (26～60 ℃ of suitable condition of enzymolysis such as moisture, temperature, be generally 42～48 ℃), pH (4～9, be generally 6～7.5), (10min～3h) etc. make the Ganoderma spore sporoderm softening and lose toughness by enzymolysis to enzymolysis time.Ganoderma spore through enzymolysis separates moisture by high speed centrifugation device or ultrafiltration membrane device.The rotating speed of centrifugal device is 3000r/min～30000r/min; Ultrafiltration membrane device filter opening molecular weight is 5000～10000.
Two, lixiviation process extracting ganoderma conidial cell wall capsule inner lipid material: select for use grease to leach the industry organic solvent with big dissolving power and higher transfer characteristic commonly used, can select for use and leach petroleum naphtha, hexane, benzene, ethylene dichloride, Ethylene Dichloride, ethanol or boiling water etc.; Can adopt grease to leach industry leaching plant commonly used during leaching extraction, can select flat-turn leacher, ring-like leacher, track type leacher, crawler belt for use---frame leacher or pot type leacher etc.; Mixed solution separates can adopt mixed solution stripping separating device, can select type equipment such as disk stripping column, laminar stripping tower, material filling type stripping tower or tubular type stripping tower for use.Can adopt following processing condition during leaching extraction: 25～100 ℃ of extraction temperatures, the most frequently used extraction temperature are 55 ℃; Solvent ratio (by weight) is (to be solvent 0.2～2.5: Ganoderma spore 1) at 0.2～2.5: 1; Extraction time is 5～150min, is generally 60～90min.In the lipid matter of ganoderma spore leaching extraction process, used solvent can be recycled.
Three, collect the lipid matter of ganoderma spore that extracts through lixiviation process, adopt filtering method,, separate the suspended substance of removing in the lipid matter of ganoderma spore as the plate-and-frame filter press of common industrial application.
The sebaceous lipid matter of ganoderma spore that is that the inventive method is extracted accounts for 6%～37% of the preceding Ganoderma spore gross weight of extraction.
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment one:
1. screen the Ganoderma spore 100kg of mature and plump.Add distilled water 100kg, 20 ℃ of water temperatures are soaked 4h.To after the Ganoderma spore that soaks is pulled drip-dry moisture out, be positioned over and impel the Ganoderma spore vernalization of sprouting in the heat and moisture preserving incubator; Keep humidity 96%, 40 ℃ of temperature, the time of sprouting is 2h.On inspection, the Ganoderma spore rate of sprouting reaches 94%.Through the supermicro mill broken wall, the microscopical determination sporoderm-broken rate reaches 99.8%.
2. with sporoderm-broken Ganoderma spore and organic solvent hexane 30kg, be positioned over leaching extraction in the flat-turn leacher, extraction temperature is 55 ℃, and extraction time is 60min; Mixed solution with leaching extraction separates through laminar stripping tower stripping then, thereby obtains lipid matter of ganoderma spore, further separates the suspended substance of removing in the lipid matter of ganoderma spore through plate-and-frame filter press.
3. will weigh through the lipid matter of ganoderma spore of leaching extraction, being sebaceous lipid matter of ganoderma spore weight is 35.8kg.Lipid matter of ganoderma spore is transparent oily matter after testing, does not have precipitation, and not oxidation has the peculiar fragrance of Ganoderma spore, free from extraneous odour.
Embodiment two:
1. screen the Ganoderma spore 100kg of mature and plump.Add chitinase 0.02kg, cellulase 0.01kg, distilled water 150kg.Enzymatic hydrolysis condition is: 43 ℃ of temperature, and pH is 6.6, enzymolysis time is 2h.Sporoderm tough and tensile in enzymolysis process loses toughness gradually.Ganoderma spore through enzymolysis separates moisture by the high speed centrifugation device, and the rotating speed of centrifugal device is 3000r/min.Through further adopting ultra micro to grind the rolling device broken wall treatment, wall breaking rate of ganoderma lucidum spores is 99.6%.
2. sporoderm-broken Ganoderma spore and organic solvent are leached petroleum naphtha 40kg, be positioned over leaching extraction in the ring-like leacher, extraction temperature is 50 ℃, and extraction time is 1.5h; Mixed solution with leaching extraction separates through the disk stripping column stripping then, thereby obtains lipid matter of ganoderma spore.Further separate the suspended substance of removing in the lipid matter of ganoderma spore through plate-and-frame filter press.
3. collect through the lipid matter of ganoderma spore of lixiviation process extraction and weigh, being sebaceous lipid matter of ganoderma spore weight is 37kg.Lipid matter of ganoderma spore is transparent oily matter after testing, does not have precipitation, and not oxidation has the peculiar fragrance of Ganoderma spore, free from extraneous odour.
Embodiment three:
1. screen the Ganoderma spore 100kg of mature and plump.
2. with Ganoderma spore and organic solvent ethylene dichloride 100kg, be positioned over leaching extraction in the track type leacher, extraction temperature is 75 ℃, and extraction time is 20min; Mixed solution with leaching extraction separates through tubular type stripping tower stripping then, thereby obtains lipid matter of ganoderma spore.Further separate the suspended substance of removing in the lipid matter of ganoderma spore through plate-and-frame filter press.
3. collect through the lipid matter of ganoderma spore of lixiviation process extraction and weigh, being sebaceous lipid matter of ganoderma spore weight is 7.5kg.Lipid matter of ganoderma spore is transparent oily matter after testing, does not have precipitation, and not oxidation has the peculiar fragrance of Ganoderma spore, free from extraneous odour.
Embodiment four:
1. screen the Ganoderma spore 100kg of mature and plump.
2. Ganoderma spore is warmed to more than 95 ℃ in 100 ℃ of baking ovens, be positioned over while hot in the ring-like leacher, add 30kg organic solvent hexane, extraction temperature is 70 ℃, and extraction time is 50min; Mixed solution with leaching extraction separates through laminar stripping tower stripping then, thereby obtains lipid matter of ganoderma spore.Further separate suspended substance in the weeding of grease metallic substance through plate-and-frame filter press.
3. collect through the lipid matter of ganoderma spore of lixiviation process extraction and weigh, being sebaceous lipid matter of ganoderma spore weight is 9.2kg.Lipid matter of ganoderma spore is transparent oily matter after testing, does not have precipitation, and not oxidation has the peculiar fragrance of Ganoderma spore, free from extraneous odour.
Embodiment five:
1. screen the Ganoderma spore 100kg of mature and plump.
2. with Ganoderma spore and organic solvent ethanol 200kg, be positioned over leaching extraction in the flat-turn leacher, extraction temperature is 35 ℃, and extraction time is 1h; Mixed solution with leaching extraction separates through laminar stripping tower stripping then, thereby obtains lipid matter of ganoderma spore.Further separate the suspended substance of removing in the lipid matter of ganoderma spore through plate-and-frame filter press.
3. collect through the lipid matter of ganoderma spore of lixiviation process extraction and weigh, being sebaceous lipid matter of ganoderma spore weight is 7.4kg.Lipid matter of ganoderma spore is transparent oily matter after testing, does not have precipitation, and not oxidation has the peculiar fragrance of Ganoderma spore, free from extraneous odour.
Embodiment six:
1. screen the Ganoderma spore 100kg of mature and plump.
2. Ganoderma spore is made popular to more than 100 ℃ through oven-baked or frying pan, with Ganoderma spore and boiling water 150kg, be positioned over leaching extraction in the flat-turn leacher while hot, extraction temperature is 100 ℃, and extraction time is 2h; Mixed solution with leaching extraction separates through laminar stripping tower stripping then, thereby obtains lipid matter of ganoderma spore.Further separate the suspended substance of removing in the lipid matter of ganoderma spore through plate-and-frame filter press.
3. collect the lipid matter of ganoderma spore of lixiviation process extraction and weigh, being sebaceous lipid matter of ganoderma spore weight is 10.2kg.Lipid matter of ganoderma spore is transparent oily matter after testing, does not have precipitation, and not oxidation has the peculiar fragrance of Ganoderma spore, free from extraneous odour.
Embodiment seven:
1. screen the Ganoderma spore 100kg of mature and plump.Add chitinase 0.02kg, distilled water 200kg.Enzymatic hydrolysis condition is: 44 ℃ of temperature, and pH is 5.9, enzymolysis time is 1.5h.Sporoderm tough and tensile in enzymolysis process loses toughness gradually.Ganoderma spore through enzymolysis separates moisture by the high speed centrifugation device, and the rotating speed of centrifugal device is 20000r/min.Shear the barreling broken wall treatment through further adopting, wall breaking rate of ganoderma lucidum spores is 99.8%.
2. with Ganoderma spore and organic solvent hexane 45kg, be positioned over leaching extraction in the pot type leacher, extraction temperature is 52 ℃, and extraction time is 80min; Mixed solution with leaching extraction separates through laminar stripping tower stripping then, thereby obtains lipid matter of ganoderma spore.Further separate the suspended substance of removing in the lipid matter of ganoderma spore through plate-and-frame filter press.
3. collect the lipid matter of ganoderma spore of lixiviation process extraction and weigh, being sebaceous lipid matter of ganoderma spore weight is 36kg.Lipid matter of ganoderma spore is transparent oily matter after testing, does not have precipitation, and not oxidation has the peculiar fragrance of Ganoderma spore, free from extraneous odour.
Embodiment eight:
1. screen the Ganoderma spore 100kg of mature and plump.Add distilled water 120kg, 37 ℃ of water temperatures are soaked 1.5h.To after the Ganoderma spore that soaks is pulled drip-dry moisture out, be positioned over and impel Ganoderma spore to be in the heat and moisture preserving incubator to sprout the vernalization phase.Humidity 98%, 42 ℃ of temperature, the time of sprouting is 1.5h.
2. Ganoderma spore and organic solvent are leached petroleum naphtha 35kg, be positioned over leaching extraction in the ring-like leacher, extraction temperature is 51 ℃, and extraction time is 65min; Mixed solution with leaching extraction separates through laminar stripping tower stripping then, thereby obtains lipid matter of ganoderma spore.Further separate the suspended substance of removing in the lipid matter of ganoderma spore through plate-and-frame filter press.
3. collect the lipid matter of ganoderma spore of lixiviation process extraction and weigh, being sebaceous lipid matter of ganoderma spore weight is 19.8kg.Lipid matter of ganoderma spore is transparent oily matter after testing, does not have precipitation, and not oxidation has the peculiar fragrance of Ganoderma spore, free from extraneous odour.
Embodiment nine:
1. screen the Ganoderma spore 100kg of mature and plump.Add cellulase 0.01kg, distilled water 250kg.Enzymatic hydrolysis condition is: 48 ℃ of temperature, and pH is 7.1, enzymolysis time is 2h.Sporoderm tough and tensile in enzymolysis process loses toughness gradually.
Ganoderma spore through enzymolysis separates moisture by the high speed centrifugation device, and the rotating speed of centrifugal device is 10000r/min.
2. will be positioned over leaching extraction in the flat-turn leacher through enzymolysis remollescent Ganoderma spore and organic solvent hexane 30kg, extraction temperature is 60 ℃, and extraction time is 70min; Mixed solution with leaching extraction separates through laminar stripping tower stripping then, thereby obtains lipid matter of ganoderma spore.Further separate the suspended substance of removing in the lipid matter of ganoderma spore through plate-and-frame filter press.
3. collect the lipid matter of ganoderma spore of lixiviation process extraction and weigh, being sebaceous lipid matter weight is 23kg.Lipid matter of ganoderma spore is transparent oily matter after testing, does not have precipitation, and not oxidation has the peculiar fragrance of Ganoderma spore, free from extraneous odour.
Claims (3)
1. the method for an extracting lipid matter of ganoderma spore by immersing extraction, it is characterized in that Ganoderma spore after pre-treatment and broken wall treatment, be dipped in the greasy organic solvent of industrial leaching commonly used, lipid matter in the Ganoderma spore is dissolved in forms mixed solution in the solvent, again mixed solution is carried out stripping and remove and to desolvate, thereby obtain lipid matter of ganoderma spore; Said pre-treatment is one of following method: 1. impel Ganoderma spore to be in through 16-49 ℃ of warm water soaking Ganoderma spore and sprout the vernalization phase, 2. add the chitinase and/or the cellulase of 0.002～2% weight ratio in Ganoderma spore, enzymolysis 10min～3h; Said broken wall treatment is to adopt mechanical micronizing, or rolls, or ground physics breaking method carries out the ultra micro broken wall.
2. in accordance with the method for claim 1, it is characterized in that used organic solvent is hexane, benzene, ethylene dichloride, Ethylene Dichloride, ethanol or boiling water.
3. according to claim 1 or 2 described methods, it is characterized in that the solvent for use and the ratio of Ganoderma spore are 0.2～2.5: 1 by weight, extraction temperature is 25～100 ℃, and extraction time is 5～150min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN00130884A CN1099455C (en) | 2000-12-25 | 2000-12-25 | Process for extracting lipid matter of ganoderma spore by immersing extraction |
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| CN1302857A CN1302857A (en) | 2001-07-11 |
| CN1099455C true CN1099455C (en) | 2003-01-22 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105886122A (en) * | 2014-12-08 | 2016-08-24 | 陈亚海 | Lucid ganoderma essential oil and preparation method thereof |
| CN104857030A (en) * | 2015-04-30 | 2015-08-26 | 黄宇明 | Wall breaking method for ganoderma lucidum spore powder and product obtained with same |
| CN106590937A (en) * | 2017-02-09 | 2017-04-26 | 陈亚海 | Process of extracting ganoderma lucidum essential oil by virtue of leaching method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1165032A (en) * | 1996-05-10 | 1997-11-19 | 中国科学院大连化学物理研究所 | Method for breaking cell wall of Ganoderma lucidum spore |
| CN1214263A (en) * | 1998-10-22 | 1999-04-21 | 湖南正清制药集团股份有限公司 | Glossy ganoderma extracting technology |
| CN1262957A (en) * | 1999-11-19 | 2000-08-16 | 中国科学院南京地理与湖泊研究所科技开发公司 | Supercritical processing method of ganoderma spore |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1165032A (en) * | 1996-05-10 | 1997-11-19 | 中国科学院大连化学物理研究所 | Method for breaking cell wall of Ganoderma lucidum spore |
| CN1214263A (en) * | 1998-10-22 | 1999-04-21 | 湖南正清制药集团股份有限公司 | Glossy ganoderma extracting technology |
| CN1262957A (en) * | 1999-11-19 | 2000-08-16 | 中国科学院南京地理与湖泊研究所科技开发公司 | Supercritical processing method of ganoderma spore |
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