CN1290554A - Extracting method for effective active matter of lucid ganoderma spore - Google Patents

Extracting method for effective active matter of lucid ganoderma spore Download PDF

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CN1290554A
CN1290554A CN 00117466 CN00117466A CN1290554A CN 1290554 A CN1290554 A CN 1290554A CN 00117466 CN00117466 CN 00117466 CN 00117466 A CN00117466 A CN 00117466A CN 1290554 A CN1290554 A CN 1290554A
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ganoderma spore
extraction
supercritical
breaking
sporoderm
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CN1114446C (en
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刘昕
钟志强
黄晓霓
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Sun Yat Sen University
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Sun Yat Sen University
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Abstract

The present invention relates to the wall breaking and supercritical CO2 fluid extracting process of obtaining effective active matter of glossy ganoderma spore. Ripe and plump glossy ganoderma spore is wall broken through medicine superfine breaking process and before breaking, chitinase or cellulase may be added to enzymolyze and soften spore wall. Wall broken glossy ganoderma spore is extracted with supercritical CO2 fluid, with the extracted oily effective active matter accounting for 37-37.6 % of the total weight of extracted glossy ganoderma spore.

Description

Extracting method for effective active matter of lucid ganoderma spore
The present invention relates to a kind of with Ganoderma spore through breaking cellular wall and supercritical CO 2Fluid (SFE-CO 2) abstraction technique obtains the method for effective active matter of lucid ganoderma spore.
Ganoderma is a Basidiomycetes Polyporaceae Ganoderma fungus.Ganoderma spore is the atomic thin avette spore of brown (6-7 * 10-12 μ m) that ejects from the cap bottom in the Ganoderma period of maturation.It is documented that Ganoderma spore has the whole hereditary active substance of Ganoderma.Because Ganoderma spore sporoderm compact structure and tough and tensile unusually, conventional extracting method is difficult to the effective active matter of extracting to Ganoderma spore, causes abundant being of the medical value of crucial importance sebaceous active substance of having of Ganoderma spore wall capsule intensive amount not to be widely used.Have document to point out, the drug effect of Ganoderma spore and value are relevant with the wall breaking technology or the sporoderm-broken rate of Ganoderma spore, the product that sporoderm-broken rate is high more, easy more being absorbed by the body.Have research to point out, to the test of Ganoderma spore active component, polysaccharide detects and is not suitable for the Ganoderma spore sample.Be subjected to extensive concern at Ganoderma spore physiologically active ingredient and anticancer mechanism and drug development thereof.
The method that the purpose of this invention is to provide a kind of high efficiency extraction effective active matter of lucid ganoderma spore is so that Ganoderma spore obtains fully, effectively utilization.
The present invention finds, in time gathers the Ganoderma spore of cultivating with log, since the freshness height, the nutrient supply abundance, the spore mature and plump adopts the conventional method breaking cellular wall, and sporoderm-broken rate is high.Experiment finds that the Ganoderma spore of breaking cellular wall can disengage the sebaceous active substance that is that is stored in the Ganoderma spore wall capsule, through supercritical CO 2Fluid extraction can obtain the sebaceous effective active matter that is up to 37.6%; And without the Ganoderma spore of breaking cellular wall, equal conditions extraction yield less than 3.5%.Zoopery and clinical test results show that effective active matter of lucid ganoderma spore has obvious inhibitory action to hepatocarcinoma and liver cancer tissue telomerase activation; The person has obvious curative effects to the HBV viral infection.As seen the effective active matter of lucid ganoderma spore that disengages of breaking cellular wall is obvious to function of tumor inhibition.
Method of the present invention is through breaking cellular wall and supercritical CO with Ganoderma spore 2Fluid extraction technology obtains effective active matter of lucid ganoderma spore, promptly utilize near critical point, the minor variations of system temperature and pressure can cause the sudden change of dissolubility generation several magnitude and the enhanced characteristic of penetration to realize separating with sporoderm being sebaceous active substance in the Ganoderma spore wall capsule, in supercritical fluid extraction equipment, finish extraction simultaneously and distill the operation of two steps, the separation efficiency height, the effective active matter of lucid ganoderma spore of extraction can keep original physiologically active, not oxidation, free from extraneous odour, no solvent residue.The Ganoderma spore extract can be applicable to oncotherapy and as having no side effect cancer therapy drug exploitation, and the inhibitor that can be used as a kind of telomerase activation is applied to clinical treatment.
The inventive method concrete steps are as follows:
One, raw material: gather Ganoderma spore and, preferably guarantee to select for use the Ganoderma spore of mature and plump through further screening.Breaking cellular wall: adopt common industrial machinery micronizing, or roll, or the physics breaking method such as grind and carry out the ultra micro breaking cellular wall, the equipment of selecting for use rolls breaking cellular wall, grinds breaking cellular wall, shear the barreling breaking cellular wall, the micronizing breaking cellular wall, ultrahigh speed airflow collision breaking cellular wall, super-voltage micro jet breaking cellular wall, type equipment such as pulverizing at ultralow temperature breaking cellular wall make breaking trachytectum of glossy ganoderma.The chitinase that can also before breaking cellular wall, in Ganoderma spore, add common commercial Application, hydrolytic enzyme such as cellulase, keep suitable condition of enzymolysis such as moisture, temperature, pH, enzymolysis time etc., make sporoderm softening and lose toughness, again through the mechanical means breaking cellular wall by enzymolysis.
Sporoderm-broken 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 10000.
Two, supercritical CO 2Fluid extraction: sporoderm-broken Ganoderma spore is put into supercritical CO 2In the extraction kettle of fluid extraction device, make it fully contact, dissolve, extract, separate with supercritical fluid, its process conditions are set as follows: extracting pressure is 5MPa~60MPa; Extraction temperature is 32 ℃~85 ℃; CO 2Fluid flow is 5kg/h~80kg/h; The extraction time is 0.5h~6h.Extraction process can add entrainer, and as ethanol, water etc., addition is for dropping into 2%~200% of material quantity.
Three, collect extract, the ethanol or the water that will add entrainer through the high speed centrifugation device separate with extract, and the rotating speed of centrifugal device is 3000r/min~30000r/min.
The sebaceous effective active matter of lucid ganoderma spore that is of the inventive method extraction accounts for 37%~37.6% 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.Through the supermicro mill breaking cellular wall, the microscopic examination sporoderm-broken rate reaches 99.6%.
2. sporoderm-broken Ganoderma spore is put into supercritical CO 2In the extraction kettle of fluid extraction device.The extraction process condition is: pressure is 35MPa; Temperature is 50 ℃; CO 2Fluid flow is 25kg/h; The extraction time is 3h.
3. extract is weighed, being sebaceous active substance weight is 37kg.Be transparent grease after testing, do not have precipitation, 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 0.01kg, cellulase 0.02kg, distilled water 200kg.Enzymatic hydrolysis condition is: 45 ℃ of temperature, and pH is 6.2, enzymolysis time is 1h.Sporoderm tough and tensile in enzymolysis process loses toughness gradually.Through further adopting the super micron mill broken wall treatment, wall breaking rate of ganoderma lucidum spores is 99.9%.
Sporoderm-broken Ganoderma spore through enzymolysis separates moisture by the high speed centrifugation device, and the rotating speed of centrifugal device is 3000r/min.
2. sporoderm-broken Ganoderma spore is put into supercritical CO 2In the extraction kettle of fluid extraction device, add 90% ethanol 10kg as entrainer, the extraction process condition is: pressure 30MPa; Temperature is 41 ℃; CO 2Fluid flow is 5kg/h; The extraction time is 5h.
3. the ethanol that will add as entrainer through the high speed centrifugation device separates with extract, and the rotating speed of centrifugal device is 3000r/min.
4. extract is weighed, being sebaceous active substance weight is 37.1kg.Be transparent grease after testing, do not have precipitation, not oxidation has the peculiar fragrance of Ganoderma spore, free from extraneous odour, no solvent residue.
Embodiment three:
1. screen the Ganoderma spore 100kg of mature and plump.Add chitinase 0.02kg, cellulase 0.01kg, distilled water 250kg, enzymatic hydrolysis condition is: 48 ℃ of temperature, pH is 6.5, enzymolysis time is 2h.Ganoderma spore sporoderm tough and tensile in enzymolysis process loses toughness gradually.Roll broken broken wall treatment through further adopting, make breaking trachytectum of glossy ganoderma.
Sporoderm-broken Ganoderma spore through enzymolysis separates moisture by the ultrafiltration membrane device.
2. sporoderm-broken Ganoderma spore is put into supercritical CO 2In the extraction kettle of fluid extraction device, the extraction process condition is: pressure is 40MPa; Temperature is 32 ℃; CO 2Fluid flow is 10kg/h; The extraction time is 4h.
3. extract is weighed, being sebaceous active substance weight is 37.3kg.Be transparent grease after testing, do not have precipitation, 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.Through ultrahigh speed airflow collision broken wall treatment, the microscopic examination sporoderm-broken rate reaches 99.6%.
2. sporoderm-broken Ganoderma spore is put into supercritical CO 2In the extraction kettle of fluid extraction device, add dehydrated alcohol 2kg as entrainer, the extraction process condition is: pressure is 10MPa; Temperature is 35 ℃; CO 2Fluid flow is 12kg/h; The extraction time is 6h.
3. the ethanol that will add as entrainer through the high speed centrifugation device separates with extract, and the rotating speed of centrifugal device is 5000r/min.
4. extract is weighed, being sebaceous active substance weight is 37.2kg.Be transparent grease after testing, do not have precipitation, not oxidation has the peculiar fragrance of Ganoderma spore, free from extraneous odour, no solvent residue.
Embodiment five:
1. screen the Ganoderma spore 100kg of mature and plump.Add chitinase 0.03kg, distilled water 250kg.Enzymatic hydrolysis condition is: 45 ℃ of temperature, and pH is 6.2, enzymolysis time is 2.5h.Sporoderm tough and tensile in enzymolysis process loses toughness gradually.Shear the barreling broken wall treatment through further adopting, wall breaking rate of ganoderma lucidum spores is 99.9%.
Sporoderm-broken Ganoderma spore through enzymolysis separates moisture by the high speed centrifugation device, and the rotating speed of centrifugal device is 15000r/min.
2. sporoderm-broken Ganoderma spore is put into supercritical CO 2In the extraction kettle of fluid extraction device, add distilled water 50kg as entrainer, the extraction process condition is: pressure is 50MPa; Temperature is 60 ℃; CO 2Fluid flow is 40kg/h; The extraction time is 2.5h.
3. the water that will add as entrainer through the high speed centrifugation device separates with extract, and the rotating speed of centrifugal device is 10000r/min.
4. extract is weighed, being sebaceous active substance weight is 37.6kg.Be transparent grease after testing, do not have precipitation, 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.Through the micronizing broken wall treatment, the microscopic examination sporoderm-broken rate reaches 99.7%.
2. sporoderm-broken Ganoderma spore is put into supercritical CO 2In the extraction kettle of fluid extraction device, add 95% ethanol 100kg as entrainer, the extraction process condition is: pressure is 55MPa; Temperature is 68 ℃; CO 2Fluid flow is 70kg/h; The extraction time is 2h.
3. the ethanol that will add as entrainer through the high speed centrifugation device separates with extract, and the rotating speed of centrifugal device is 20000r/min.
4. extract is weighed, being sebaceous active substance weight is 37.5kg.Be transparent grease after testing, do not have precipitation, not oxidation has the peculiar fragrance of Ganoderma spore, free from extraneous odour, no solvent residue.
Embodiment seven:
1. screen the Ganoderma spore 100kg of mature and plump.Add cellulase 0.03kg, distilled water 200kg.Enzymatic hydrolysis condition is: 40 ℃ of temperature, and pH is 5.8, enzymolysis time is 1.5h.Sporoderm tough and tensile in enzymolysis process loses toughness gradually.Through rolling break process, wall breaking rate of ganoderma lucidum spores is 99.8%.
Sporoderm-broken Ganoderma spore through enzymolysis separates moisture by the high speed centrifugation device, and the rotating speed of centrifugal device is 20000r/min.
2. sporoderm-broken Ganoderma spore is put into supercritical CO 2In the extraction kettle of fluid extraction device, the extraction process condition is: pressure is 60MPa; Temperature is 75 ℃; CO 2Fluid flow is 80kg/h; The extraction time is 0.5h.
3. extract is weighed, being sebaceous active substance weight is 37.4kg.Be transparent grease after testing, do not have precipitation, not oxidation has the peculiar fragrance of Ganoderma spore, free from extraneous odour, no solvent residue.
Embodiment eight:
1. screen the Ganoderma spore 100kg of mature and plump.Through shearing the barreling broken wall treatment, the microscopic examination sporoderm-broken rate reaches 99.9%.
Sporoderm-broken Ganoderma spore through enzymolysis separates moisture by the high speed centrifugation device, and the rotating speed of centrifugal device is 30000r/min.
2. sporoderm-broken Ganoderma spore is put into supercritical CO 2In the extraction kettle of fluid extraction device, add 90% ethanol 100kg as entrainer, the extraction process condition is: pressure is 15MPa; Temperature is 48 ℃; CO 2Fluid flow is 25kg/h; The extraction time is 2h.
3. the ethanol that will add as entrainer through the high speed centrifugation device separates with extract, and the rotating speed of centrifugal device is 25000r/min.
4. extract is weighed, being sebaceous active substance weight is 37.5kg.Be transparent grease after testing, do not have precipitation, not oxidation has the peculiar fragrance of Ganoderma spore, free from extraneous odour, no solvent residue.
Embodiment nine:
1. screen the Ganoderma spore 100kg of mature and plump.Add chitinase 0.01kg, cellulase 0.01kg, distilled water 220kg.Enzymatic hydrolysis condition is: 45 ℃ of temperature, and pH is 7.3, enzymolysis time is 1.5h.Sporoderm tough and tensile in enzymolysis process loses toughness gradually.Through adopting ultra micro to roll broken wall treatment, wall breaking rate of ganoderma lucidum spores is 99.9%.
Sporoderm-broken Ganoderma spore through enzymolysis separates moisture by the ultrafiltration membrane device.
2. sporoderm-broken Ganoderma spore is put into supercritical CO 2In the extraction kettle of fluid extraction device, add distilled water 10kg as entrainer, the extraction process condition is: pressure is 5MPa; Temperature is 85 ℃; CO 2Fluid flow is 35kg/h; The extraction time is 1.5h.
3. the water that will add as entrainer through the high speed centrifugation device separates with extract, and the rotating speed of centrifugal device is 30000r/min.
4. extract is weighed, being sebaceous active substance weight is 37.1kg.Be transparent grease after testing, do not have precipitation, not oxidation has the peculiar fragrance of Ganoderma spore, free from extraneous odour.
Embodiment ten:
1. screen the Ganoderma spore 100kg of mature and plump.Handle through super-voltage micro jet, the microscopic examination sporoderm-broken rate reaches 99.9%.
2. sporoderm-broken Ganoderma spore is put into supercritical CO 2In the extraction kettle of fluid extraction device, add 80% ethanol 200kg as entrainer, the extraction process condition is: pressure is 14MPa; Temperature is 40 ℃; CO 2Fluid flow is 12kg/h; The extraction time is 0.5h.
3. the ethanol that will add as entrainer through the high speed centrifugation device separates with extract, and the rotating speed of centrifugal device is 6000r/min.
4. extract is weighed, being sebaceous active substance weight is 37.4kg.Be transparent grease after testing, do not have precipitation, not oxidation has the peculiar fragrance of Ganoderma spore, free from extraneous odour, no solvent residue.

Claims (6)

1. an extracting method for effective active matter of lucid ganoderma spore is characterized in that Ganoderma spore is through breaking cellular wall, supercritical CO 2Fluid extraction and extract separation circuit are handled.
2. the method for claim 1 is characterized in that selecting for use the Ganoderma spore of mature and plump.
3. the method for claim 1 adopts mechanical micronizing, or rolls when it is characterized in that breaking cellular wall, or ground physics breaking method carries out the ultra micro breaking cellular wall.
4. the method for claim 1 adds chitinase and/or cellulase when it is characterized in that breaking cellular wall.
5. the method for claim 1 is characterized in that supercritical CO 2Fluid extraction pressure is 5MPa~60MPa, and extraction temperature is 32 ℃~85 ℃, CO 2Fluid flow is 5kg/h~80kg/h, and the extraction time is 0.5h~6h.
6. the method for claim 1 is characterized in that at supercritical CO 2The fluid extraction process adds entrainer ethanol and/or water, and addition is for dropping into 2%~200% of material quantity.
CN 00117466 2000-10-09 2000-10-09 Extracting method for effective active matter of lucid ganoderma spore Expired - Lifetime CN1114446C (en)

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1245235A3 (en) * 2001-03-19 2002-10-09 Xin Liu Method for extracting oleaginous substances from ganoderma lucidum spores
CN100339089C (en) * 2003-10-14 2007-09-26 上海中祥生物制品有限公司 Method for extracting ganoderma lucidum oil from ganoderma lucidum mycelium
WO2007134548A1 (en) * 2006-05-24 2007-11-29 Guangdong Yuewei Edible Fungi Technology Co. Ltd A process for preparing ganoderma spore oil
CN101028305B (en) * 2007-03-23 2010-08-25 卢昶年 Ganoderic spore extract and its production
CN102204942A (en) * 2011-05-24 2011-10-05 黑龙江大学 Method for extracting corylus heterophylla leaf flavone
CN101176548B (en) * 2007-11-30 2012-05-09 华南理工大学 Method for preparing low acid value ganoderma lucidum spore oil
CN103351941A (en) * 2013-06-17 2013-10-16 浙江龙泉佳宝生物科技有限公司 Supercritical CO2 variable-temperature variable-pressure extraction method of lucid ganoderma spore oil
CN104137979A (en) * 2014-07-29 2014-11-12 桂林实力科技有限公司 Fructus momordicae aspartame and preparation method thereof
CN105219647A (en) * 2015-10-23 2016-01-06 南京中医药大学 A kind of wall-breaking method of Ganoderma spore
CN112779086A (en) * 2020-12-18 2021-05-11 江苏滋补堂药业有限公司 Method for removing peroxide value of ganoderma lucidum spore oil
CN113684088A (en) * 2020-05-18 2021-11-23 嘉必优生物技术(武汉)股份有限公司 Microbial oil extraction method and microbial oil obtained by same

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CN1308011C (en) * 2003-12-22 2007-04-04 中国科学院微生物研究所 Method for extracting ganoderma lucidum spore fat soluble active substance and its specified instrument for preparation

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1245235A3 (en) * 2001-03-19 2002-10-09 Xin Liu Method for extracting oleaginous substances from ganoderma lucidum spores
CN100339089C (en) * 2003-10-14 2007-09-26 上海中祥生物制品有限公司 Method for extracting ganoderma lucidum oil from ganoderma lucidum mycelium
WO2007134548A1 (en) * 2006-05-24 2007-11-29 Guangdong Yuewei Edible Fungi Technology Co. Ltd A process for preparing ganoderma spore oil
CN101028305B (en) * 2007-03-23 2010-08-25 卢昶年 Ganoderic spore extract and its production
CN101176548B (en) * 2007-11-30 2012-05-09 华南理工大学 Method for preparing low acid value ganoderma lucidum spore oil
CN102204942B (en) * 2011-05-24 2012-12-05 黑龙江大学 Method for extracting corylus heterophylla leaf flavone
CN102204942A (en) * 2011-05-24 2011-10-05 黑龙江大学 Method for extracting corylus heterophylla leaf flavone
CN103351941A (en) * 2013-06-17 2013-10-16 浙江龙泉佳宝生物科技有限公司 Supercritical CO2 variable-temperature variable-pressure extraction method of lucid ganoderma spore oil
CN103351941B (en) * 2013-06-17 2015-06-17 浙江龙泉佳宝生物科技有限公司 Supercritical CO2 variable-temperature variable-pressure extraction method of lucid ganoderma spore oil
CN104137979A (en) * 2014-07-29 2014-11-12 桂林实力科技有限公司 Fructus momordicae aspartame and preparation method thereof
CN104137979B (en) * 2014-07-29 2015-12-02 桂林实力科技有限公司 A kind of mangosteen sweetener and preparation method thereof
CN105219647A (en) * 2015-10-23 2016-01-06 南京中医药大学 A kind of wall-breaking method of Ganoderma spore
CN113684088A (en) * 2020-05-18 2021-11-23 嘉必优生物技术(武汉)股份有限公司 Microbial oil extraction method and microbial oil obtained by same
CN113684088B (en) * 2020-05-18 2024-06-11 嘉必优生物技术(武汉)股份有限公司 Microbial oil extraction method and microbial oil obtained by same
CN112779086A (en) * 2020-12-18 2021-05-11 江苏滋补堂药业有限公司 Method for removing peroxide value of ganoderma lucidum spore oil

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