CN104845732A - Method for efficiently extracting ganoderma lucidum spores oil by using subcritical mixed solvent - Google Patents
Method for efficiently extracting ganoderma lucidum spores oil by using subcritical mixed solvent Download PDFInfo
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- CN104845732A CN104845732A CN201510226126.5A CN201510226126A CN104845732A CN 104845732 A CN104845732 A CN 104845732A CN 201510226126 A CN201510226126 A CN 201510226126A CN 104845732 A CN104845732 A CN 104845732A
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Abstract
The invention provides a method for efficiently extracting ganoderma lucidum spores oil by using a subcritical mixed solvent. The method comprises the following steps: adding ganoderma lucidum spores powder and distilled water, and making into ganoderma lucidum spores powder particles by using a granulator, wherein the mass ratio of the ganoderma lucidum spores powder to the distilled water is 10:1, and the ganoderma lucidum spores powder is subjected to wall breakage; placing the ganoderma lucidum spores powder particles into a low temperature freeze dryer for drying and dehydration; placing the ganoderma lucidum spores powder particles into an extracting bag, putting the extracting bag into a separation pot I, sealing the separation pot I and vacuuming to -0.1MPa, adding an extraction agent to completely immerse the ganoderma lucidum spores powder particles in the extraction agent, and performing extraction for 1-3 hours so as to obtain extract, wherein the pressure is controlled to be 0.2-0.5 MPa, and the temperature is controlled to be 20-25 DEG C; loading the extract into a separation pot II, heating for distillation at the temperature of 70-80 DEG C, and separating coarse ganoderma lucidum spores oil; performing vacuum thin film evaporation on the coarse ganoderma lucidum spores oil so as to obtain the product. The method provided by the invention is non-poisonous, environment-friendly and pollution-free; the activity of the extract can be well preserved, the operating cost is low, the extracting efficiency is high, and large-scale production can be realized.
Description
Technical field
The present invention is specifically related to the method for the efficient Ganoderma Lucidum Spores Oil Extracted of a kind of subcritical mixed solvent.
Background technology
Ganoderma Basidiomycetes, polyporaceae, be China traditional strengthen the body resistance to consolidate the constitution, the rare Chinese medicine of strengthening by means of tonics.Have the good reputation of " celestial grass ", have the medical, edible history of more than 5000 year in China.Glossy ganoderma all has suitable Species distributing at different ecological environment, and constituted abundant glossy ganoderma monoid, wherein especially red ganoderma drug action is the most outstanding.Ganoderma spore is the sexual cell that glossy ganoderma mature period constantly ejects from cap, and these fine sporozoites are the seeds of breeding glossy ganoderma of future generation, and it is whole genetic material of glossy ganoderma and breeds the necessary nutrition elite of glossy ganoderma new life.Ganoderma spore has tough and tensile shell, is not dissolved in water, hydrochloric acid in gastric juice etc., becomes the major obstacle of its effective constituent of absorption of human body; Usually super-fine powder broken wall or enzymolysis wall breaking technology is adopted to carry out broken wall to Ganoderma spore in processing.Current broken wall ultra-micro powder wall-breaking technique is comparatively ripe, can realize suitability for industrialized production.
Ganoderma spore powder contains whole genetic activities materials of glossy ganoderma, is the elite of glossy ganoderma, has the effects such as antitumor, hypoglycemic and strengthening immunity.Ganoderma spore oil is the essential ingredient extracted from Ganoderma spore, contains the compositions such as the triterpene substance in Ganoderma spore, fatty acid, ergosterol class, polyose, is the aggregate of Ganoderma spore effective constituent, has multiple physiologically active.In recent years, Ganoderma spore oil has been developed to as various high-grade healthcare products, has very important medical value and economic worth.
Main component in sporoderm-broken Ganoderma spore is triterpene compound and lipid acid etc., is lipotropy hydrocarbon polymer and lipoid organic compound, can be dissolved in CHCl
3, CH
3the organic solvents such as OH.The most frequently used extracting method of Ganoderma spore oil comprises organic solvent extraction and supercritical CO
2extraction.Supercritical CO
2fluid has better solvability to Ganoderma spore effective constituent, CO
2have colourless, tasteless, nontoxic, nonflammable explosive feature, and no solvent residue problem after extraction, so supercritical CO
2fluid extraction process quilt is widely used in large-scale production.But due to supercritical CO
2extraction process needs to complete under comparatively extreme condition, and such as operation pressure needs to reach 30MPa-35MPa, and extraction time is longer.This technique can cause destruction to a certain degree to the activeconstituents of Ganoderma spore in whole preparation process.In prior art, adopt supercritical CO
2the patent report of Ganoderma Lucidum Spores Oil Extracted is more, in Chinese patent CN1194079C, Ganoderma spore powder is expanded through bulking machine, granulation, the mass transfer effect in extraction process can be improved, increase oil yield, but adopt puffing technique temperature higher, oxidation and the process of spoilage of lipid in spore powder can be accelerated, disadvantageous effect is brought to the quality of oil.Chinese patent CN1094766C discloses a kind of supercritical CO of Ganoderma spore oil
2extraction working method, relate to the mixture of Ganoderma spore and water, gelatin or starch is carry out supercritical extraction after tackiness agent pelletizing forming, extraction temperature, the pressure of the method are wider, be difficult to grasp processing condition during production and obtain high purity spore oil product, extraction time also reaches 35 hours simultaneously, is difficult to really realize industrialization.
From the development trend of Ganoderma spore oil relevant healthcare food, future expands just increasingly to the demand of Ganoderma spore oil raw material, exploitation one rapidly and efficiently can extract Ganoderma spore oil, the method of functional component activity in Ganoderma spore oil can be kept again preferably, there is significant realistic meaning and using value.
Summary of the invention
The technical problem to be solved in the present invention, is the method providing the efficient Ganoderma Lucidum Spores Oil Extracted of a kind of subcritical mixed solvent.
The present invention is achieved in that the method for the efficient Ganoderma Lucidum Spores Oil Extracted of a kind of subcritical mixed solvent, comprises the following steps:
(1) Ganoderma spore powder in mass ratio: distilled water=10:1, adds the Ganoderma spore powder through broken wall and distilled water in nodulizer, makes 10 ~ 20 object Ganoderma spore powder particles through nodulizer;
(2) by Ganoderma spore powder particles, low-temperature freeze-drying machine drying and dehydrating is placed in;
(3) dried Ganoderma spore powder particles is loaded bag for extracting, be placed in airtight stainless steel separation reactor I, close separation reactor I and be evacuated to-0.1MPa, extraction agent is added to complete submergence Ganoderma spore powder particles in separation reactor I, carry out extracting operation, control pressure is 0.2 ~ 0.5MPa, and temperature is 20 ~ 25 DEG C, extraction time is 1 ~ 3h, obtains extracting solution;
Wherein, every 1kg Ganoderma spore powder particles adds 2 ~ 3kg extraction agent, and it is 5:1 normal butane and dehydrated alcohol that described extraction agent comprises volume ratio;
(4) described extracting solution is squeezed into separation reactor I I, at 70 ~ 80 DEG C, add thermal distillation, reclaim extraction agent, isolate thick Ganoderma spore oil;
(5) carry out Vacuum film evaporation with Rotary Evaporators to thick Ganoderma spore oil, control vacuum tightness-0.1MPa, Heating temperature 70 ~ 80 DEG C, until the residual quantity of normal butane is less than 1ppm, namely obtains Ganoderma spore oil production.
Preferably, in described step (2), Ganoderma spore powder particle drying dewaters to water ratio lower than 5.0%.
Preferably, described ethanol is food grade.
The invention has the advantages that: there is extraction conditions gentleness, the advantages such as save the functional active components in Ganoderma spore oil preferably, working pressure is little, and Extracting temperature is low, and extraction time is short; Have nontoxic, harmless, environmental protection, pollution-free, do not destroy extract, be not oxidized, can retain the activity of extract preferably, product is easy to be separated with extraction agent, and running cost is low, and extraction efficiency is high, the advantage that can accomplish scale production.
Embodiment
A method for the efficient Ganoderma Lucidum Spores Oil Extracted of subcritical mixed solvent, comprises the following steps:
(1) Ganoderma spore powder in mass ratio: distilled water=10:1, adds the Ganoderma spore powder through broken wall and distilled water in nodulizer, makes 10 ~ 20 object Ganoderma spore powder particles through nodulizer;
(2) by Ganoderma spore powder particles, low-temperature freeze-drying machine drying and dehydrating is placed in water ratio lower than 5%;
(3) dried Ganoderma spore powder particles is loaded bag for extracting, be placed in airtight stainless steel separation reactor I, close separation reactor I and be evacuated to-0.1MPa, in separation reactor I, add extraction agent to complete submergence Ganoderma spore powder particles, carry out extracting operation, control pressure is 0.2 ~ 0.5MPa, temperature is 20 ~ 25 DEG C, make extraction agent reach subcritical state, extraction time is 1 ~ 3h, obtains extracting solution;
Wherein, every 1kg Ganoderma spore powder particles adds 2 ~ 3kg extraction agent, and it is 5:1 normal butane and dehydrated alcohol that described extraction agent comprises volume ratio;
(4) described extracting solution is squeezed into separation reactor I I, at 70 ~ 80 DEG C, add thermal distillation, reclaim extraction agent, isolate thick Ganoderma spore oil;
(5) carry out Vacuum film evaporation with Rotary Evaporators to thick Ganoderma spore oil, control vacuum tightness-0.1MPa, Heating temperature 70 ~ 80 DEG C, until the residual quantity of normal butane is less than 1ppm, namely obtains Ganoderma spore oil production.Described ethanol is food grade, and a small amount of remaining does not affect security in the product.
Embodiment one
A. get the Ganoderma spore powder of 10kg broken wall, add 1kg water and make 10 order particles through nodulizer, and dewater extremely lower than 5% in freeze drier;
B. Ganoderma spore powder particles is packed, be placed in and put into airtight stainless steel separating still I and be evacuated to-0.1MPa, extraction agent is done with normal butane-dehydrated alcohol mixed solvent, normal butane and dehydrated alcohol quality are respectively 20kg and 5kg, controlling to extract pressure is 0.3MPa, extraction temperature is 25 DEG C, and extraction time is 1h, obtains extracting solution;
C. extracting solution is squeezed into separation reactor I I, add thermal distillation, reclaim extraction agent, control Heating temperature 80 DEG C, isolate thick Ganoderma spore oil 3.5kg, oil yield 35%;
D. with Rotary Evaporators, Vacuum film evaporation is carried out to thick Ganoderma spore oil, remove residual extractant further, control vacuum tightness is-0.1MPa, Heating temperature 80 DEG C, to Ganoderma spore oil, the residual quantity of normal butane is less than 1ppm, and the residual quantity of ethanol is less than 10ppm, obtains the Ganoderma spore oil 3.3kg refined, total oil yield 33%, Ganoderma total triterpenes content is 36.3%.
Embodiment two
This part and embodiment one difference are:
B. normal butane and dehydrated alcohol quality are respectively 24kg and 6kg, and controlling to extract pressure is 0.5MPa, and extraction temperature is 20 DEG C, and extraction time is 3h;
C. control Heating temperature 70 DEG C, isolate thick Ganoderma spore oil 3.5kg, oil yield 32%;
D. Heating temperature 70 DEG C, obtains the Ganoderma spore oil 3.3kg refined, total oil yield 31%, and Ganoderma total triterpenes content is 36.6%.
Embodiment three
This part and embodiment one difference are:
B. normal butane and dehydrated alcohol quality are respectively 16kg and 4kg, and controlling to extract pressure is 0.2MPa, and extraction temperature is 23 DEG C, and extraction time is 2h;
C. control Heating temperature 75 DEG C, isolate thick Ganoderma spore oil 3.5kg, oil yield 32.5%;
D. Heating temperature 75 DEG C, obtains the Ganoderma spore oil 3.3kg refined, total oil yield 31%, and Ganoderma total triterpenes content is 36.1%.
The present invention has the following advantages:
1, extraction efficiency is high: the present invention adopts subcritical normal butane-alcohol mixed solvent to be that extraction agent extracts Ganoderma spore oil from Ganoderma spore powder with cellular wall broken, relative to conventional supercritical fluid CO
2extraction process has increased substantially extraction efficiency, and extraction yield is up to 33%.
2, its lytic activity composition is extracted high: extraction conditions of the present invention is relatively gentle, and pressure is no more than 0.5MPa, saves the functional active components in Ganoderma spore oil preferably, Ganoderma total triterpenes content >=30% in its extraction product Ganoderma spore oil.
3, simple for process: relative to traditional supercritical CO
2extraction process, the features such as it is little that the present invention has working pressure, and Extracting temperature is low, extraction time is short; Have nontoxic, harmless, environmental protection, pollution-free, do not destroy extract, be not oxidized, can retain the activity of extract preferably, product is easy to be separated with extraction agent; Running cost is low, and extraction efficiency is high, can accomplish scale production.
Claims (3)
1. a method for the efficient Ganoderma Lucidum Spores Oil Extracted of subcritical mixed solvent, is characterized in that: comprise the following steps:
(1) Ganoderma spore powder in mass ratio: distilled water=10:1, adds the Ganoderma spore powder through broken wall and distilled water in nodulizer, makes 10 ~ 20 object Ganoderma spore powder particles through nodulizer;
(2) by Ganoderma spore powder particles, low-temperature freeze-drying machine drying and dehydrating is placed in;
(3) dried Ganoderma spore powder particles is loaded bag for extracting, be placed in airtight stainless steel separation reactor I, close separation reactor I and be evacuated to-0.1MPa, extraction agent is added to complete submergence Ganoderma spore powder particles in separation reactor I, carry out extracting operation, control pressure is 0.2 ~ 0.5MPa, and temperature is 20 ~ 25 DEG C, extraction time is 1 ~ 3h, obtains extracting solution;
Wherein, every 1kg Ganoderma spore powder particles adds 2 ~ 3kg extraction agent, and it is 5:1 normal butane and dehydrated alcohol that described extraction agent comprises volume ratio;
(4) described extracting solution is squeezed into separation reactor I I, at 70 ~ 80 DEG C, add thermal distillation, reclaim extraction agent, isolate thick Ganoderma spore oil;
(5) carry out Vacuum film evaporation with Rotary Evaporators to thick Ganoderma spore oil, control vacuum tightness-0.1MPa, Heating temperature 70 ~ 80 DEG C, namely obtains Ganoderma spore oil production.
2. the method for the efficient Ganoderma Lucidum Spores Oil Extracted of subcritical mixed solvent as claimed in claim 1, is characterized in that: in described step (2), and Ganoderma spore powder particle drying dewaters to water ratio lower than 5.0%.
3. the method for the efficient Ganoderma Lucidum Spores Oil Extracted of subcritical mixed solvent as claimed in claim 1, is characterized in that: described ethanol is food grade.
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Cited By (7)
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| CN106381220A (en) * | 2016-10-19 | 2017-02-08 | 南京希元生物医药科技有限公司 | Preparation process of ganoderma lucidum spores oil |
| CN107158043A (en) * | 2017-04-10 | 2017-09-15 | 浙江寿仙谷医药股份有限公司 | One kind removes wall lucidum spore powder, particle and preparation method thereof |
| CN108853153A (en) * | 2018-09-21 | 2018-11-23 | 贵州灵康士生物科技有限公司 | A kind of preparation method of G. lucidum spores Softgel |
| CN114917261A (en) * | 2022-05-30 | 2022-08-19 | 安徽芝神堂药业有限公司 | Production process of ganoderma lucidum spore oil extract for adjuvant therapy of tumors |
| CN115141679A (en) * | 2022-06-20 | 2022-10-04 | 福建仙芝楼生物科技有限公司 | Ganoderma spore oil with natural flavor |
| CN115261122A (en) * | 2022-09-01 | 2022-11-01 | 杭州香芝生物科技有限公司 | Method for subcritical fluid extraction of ganoderma lucidum spore compound oil |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106318616A (en) * | 2016-10-19 | 2017-01-11 | 南京希元生物医药科技有限公司 | Ganoderma lucidum spores oil |
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| CN108853153A (en) * | 2018-09-21 | 2018-11-23 | 贵州灵康士生物科技有限公司 | A kind of preparation method of G. lucidum spores Softgel |
| CN114917261A (en) * | 2022-05-30 | 2022-08-19 | 安徽芝神堂药业有限公司 | Production process of ganoderma lucidum spore oil extract for adjuvant therapy of tumors |
| CN115141679A (en) * | 2022-06-20 | 2022-10-04 | 福建仙芝楼生物科技有限公司 | Ganoderma spore oil with natural flavor |
| CN115141679B (en) * | 2022-06-20 | 2023-09-15 | 福建仙芝楼生物科技有限公司 | Ganoderma lucidum spore oil with natural flavor |
| CN115261122A (en) * | 2022-09-01 | 2022-11-01 | 杭州香芝生物科技有限公司 | Method for subcritical fluid extraction of ganoderma lucidum spore compound oil |
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Application publication date: 20150819 |