CN105477024A - Compound extraction method of ganoderma triterpenes and triterpenoid saponin with high concentrations - Google Patents
Compound extraction method of ganoderma triterpenes and triterpenoid saponin with high concentrations Download PDFInfo
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- CN105477024A CN105477024A CN201510957448.7A CN201510957448A CN105477024A CN 105477024 A CN105477024 A CN 105477024A CN 201510957448 A CN201510957448 A CN 201510957448A CN 105477024 A CN105477024 A CN 105477024A
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/06—Fungi, e.g. yeasts
- A61K36/07—Basidiomycota, e.g. Cryptococcus
- A61K36/074—Ganoderma
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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Abstract
The invention discloses a compound extraction method of ganoderma triterpenes and triterpenoid saponin with high concentrations, relating to an extraction technology for active ingredients of lucid ganoderma. The compound extraction method comprises six steps of including smashing, reduction treatment, freeze thawing, wall breaking, supercritical CO2 extraction and freeze drying. According to the compound extraction method, before the supercritical CO2 extraction is carried out, lucid ganoderma powder is subjected to reduction, repetitive freeze-thawing and wall breaking treatment, ascorbic acid is adopted for carrying out antioxidation treatment on lucid ganoderma powder, so that the oxidation of ganoderma triterpenes and triterpenoid saponin substance is prevented, further, the compact structure of the sporocarp of lucid ganoderma is completely broken in combination with the repetitive freeze-thawing and ultrasonic wall breaking technologies, so that the bioactive components with high concentrations are guaranteed, and in addition, the industrial production cost is low, the implementation is convenient, and the market prospect is very hopeful.
Description
Technical field
The present invention relates to effective component of glossy ganoderma extractive technique, particularly a kind of high concentration Ganoderma triterpenoids and triterpene saponin composite extracting method.
Background technology
Ganoderma is precious also known as Lin Zhongling, fine jade, and profile is umbrella, cap kidney shape, semicircle or subcircular, is the sporophore of On Polyporaceae Ganoderma.There is effect of invigorating QI and tranquilization, relieving cough and asthma, for dizzy sleeplessness, shortness of breath and palpitation, neurasthenia, asthenia cough with asthma, life lengthening.Ganoderma in the medicinal history of state-owned more than one thousand years, the growth from 35 years old of king of medicine Sun Simiao takes Ganoderma, within 101 years old, dies without known cause, with oneself all one's life witness Ganoderma the road of longevity.Main containing aminoacid, polypeptide, protein, fungal lysozyme and saccharide, ergosterol, triterpenes, coumarin glycoside, volatile oil, stearic acid, benzoic acid, alkaloid, vitamin B2 and C etc. in Ganoderma; Spore is also containing mannitol, trehalose.Triterpenoid compound is one of the primary chemical and active ingredient of Ganoderma.In Ganoderma, contained triterpenoid compound has significant especially physiologically active.That studies Ganoderma along with modern science gos deep into, to so far, altogether be separated to more than 350 and plant chemical composition, wherein many chemical compositions at antitumor, protect the liver, blood sugar lowering, blood fat reducing, enhancing mononuclear phagocyte system and NK cell function, strengthen humoral immune function, anti-radiation, analgesia, calmness, anti-ageing wait for a long time in show stronger activity.At present, the extracting method of known ganoderma lucidum triterpene compounds can be divided into organic solvent extraction and supercritical CO
2extraction, organic solvent extraction extracts Ganoderma medical material or spore powder with the organic reagent such as chloroform or methanol and obtains crude extract, again with saturated sodium bicarbonate solution extraction taking-up acid ingredient wherein, hcl acidifying, chloroform extraction go on a tour from acid ingredient, obtain the triterpenes components that content is higher, this method usually needs longer extraction time and consumes a large amount of Extraction solvent, and the use of a large amount of organic solvent simultaneously can bring adverse influence to human body and environment; Therefore present most enterprise with good conditionsi all adopts supercritical CO
2extraction, supercritical CO
2abstraction technique is the CO with supercriticality
2for extractant, from liquid or solid, extract effective ingredient and carry out the method that is separated, the method to many materials particularly low-polarity component there is good permeability and stronger solvability, compared with conventional solvent extraction, have applied widely, to material composition without destruction, to advantages such as product and environmental nonpollution, extraction efficiency are high and easy to operate, application number be 201410243422.1 patent of invention disclose a kind of ganoderma lucidum triterpene and the multiple extraction process of polysaccharide effective ingredient and health food thereof, by supercritical CO
2extracting ganoderma triterpenes components, the compositions such as water extraction ganoderan, allotment mixing granulation, metering filled capsules, it is obtained to pack these steps, and product of the present invention is rich in the essential ingredient of Ganoderma and multiple bioactive ingredients; Application number be 200710094452.0 patent of invention disclose fast preparation method of a kind of ganoderma lucidum triterpene compounds and products thereof, key step comprises CO
2supercritical liquid extraction technique extracts, extract dissolve with ethanol, the enrichment of sephadex chromatography post, purification, concentrating under reduced pressure, and preparation method fast, simply, in product, effective triterpenoid compound kind and content are all significantly improved.But above-mentioned supercritical CO
2all there is a defect in the method that abstraction technique extracts ganoderma lucidum triterpene compounds, does not namely carry out pretreatment to Ganoderma, adds supercritical CO after directly being pulverized by Ganoderma sporophore
2control relevant parameter in the extraction kettle of extraction equipment to extract, and Ganoderma sporophore is made up of main components such as cellulose, hemicellulose and lignins, close structure, thus direct the Ganoderma powder of simple pulverization process is carried out CO
2supercritical extraction, its yield also must be influenced.Therefore needing that exploitation is a kind of badly can the method for high efficiency extraction ganoderma lucidum triterpene compounds.
Summary of the invention
The invention provides a kind of high concentration Ganoderma triterpenoids and triterpene saponin composite extracting method, overcome existing market supercritical CO
2abstraction technique does not carry out pretreatment to Ganoderma when extracting ganoderma lucidum triterpene compounds, adds supercritical CO after directly being pulverized by Ganoderma sporophore
2control relevant parameter in the extraction kettle of extraction equipment to extract, and Ganoderma sporophore is made up of main components such as cellulose, hemicellulose and lignins, close structure, thus direct the Ganoderma powder of simple pulverization process is carried out CO
2supercritical extraction, the affected defect of its yield, the invention provides a kind of technique simple, the suitable extracting method that can extract high concentration Ganoderma triterpenoids and triterpene saponin promoted.
The present invention is achieved through the following technical solutions: a kind of high concentration Ganoderma triterpenoids and triterpene saponin composite extracting method, comprise the steps:
(1) pulverize: choose top grade Ganoderma, cut into slices, after pulverizing, also cross 100 mesh sieves;
(2) reduction treatment: the Ganoderma powder that step (1) obtains is added reduction treatment 1-2h in 1% ascorbic acid solution and namely obtain reduction Ganoderma mixture, the ratio of described Ganoderma powder and 1% ascorbic acid solution is m:v is 1:3-5;
(3) freeze thawing: reduction Ganoderma mixture step (2) handled well is placed in freeze thawing case, adds liquid nitrogen multigelation 6-8 time;
(4) breaking cellular wall: use the reduction Ganoderma mixture of 40% alcoholic solution to step (3) freeze thawing treatment to carry out ultrasonic air alveolation breaking cellular wall, the supersonic frequency of ultrasonic output 400-440W, employing 50-60kHz, supersound process 30-45min, stagnate 8-12min, supersound process 28-32min again, concentrated ultrasonic liquid obtains breaking cellular wall and concentrates lucidum liquid;
(5) supercritical CO
2extraction: get breaking cellular wall that step (4) obtains and concentrate lucidum liquid and carry out supercritical CO
2extraction, extraction conditions is pressure 14MPa, temperature 30-32 DEG C, dynamic extraction time 100-110min, CO
2flow 1mL/min, counterbalance valve temperature 45 C, collects extract classification;
(6) lyophilization.
Compared with prior art, the present invention has following outstanding advantages and effect: invention applies at present state-of-the-art supercritical CO in the world
2abstraction technique obtains the effective bioactive substance of Ganoderma, is carrying out supercritical CO
2respectively Ganoderma powder is reduced before extraction, multigelation and broken wall treatment, ascorbic acid is adopted to carry out anti-oxidant treatment to prevent the Oxidation of Ganoderma triterpenoids and triterpene saponin material to Ganoderma powder, and then in conjunction with multigelation and ultrasonication technology by Ganoderma sporophore closely structure thoroughly destroy thus ensure that the bioactive ingredients of high concentration, and industrial production cost is low, be convenient to implement, market prospect is very optimistic.
Detailed description of the invention
Following Examples further illustrates the present invention, but should as restriction of the present invention:
Embodiment 1: a kind of high concentration Ganoderma triterpenoids and triterpene saponin composite extracting method, comprise the steps:
(1) pulverize: choose top grade Ganoderma, cut into slices, after pulverizing, also cross 100 mesh sieves;
(2) reduction treatment: take Ganoderma powder that 300g step (1) obtains and be added to reduction treatment 2h in 1% ascorbic acid solution of 1200ml and namely obtain reduction Ganoderma mixture;
(3) freeze thawing: reduction Ganoderma mixture step (2) handled well is placed in freeze thawing case, adds liquid nitrogen multigelation 8 times;
(4) breaking cellular wall: use the reduction Ganoderma mixture of 40% alcoholic solution to step (3) freeze thawing treatment to carry out ultrasonic air alveolation breaking cellular wall, the supersonic frequency of ultrasonic output 440W, employing 50kHz, supersound process 35min, stagnate 10min, supersound process 28min again, concentrated ultrasonic liquid obtains breaking cellular wall and concentrates lucidum liquid;
(5) supercritical CO
2extraction: get breaking cellular wall that step (4) obtains and concentrate lucidum liquid and carry out supercritical CO
2extraction, extraction conditions is pressure 14MPa, temperature 30 DEG C, dynamic extraction time 100min, CO
2flow 1mL/min, counterbalance valve temperature 45 C, collects extract classification;
(6) lyophilization.
Embodiment 2: a kind of high concentration Ganoderma triterpenoids and triterpene saponin composite extracting method, comprise the steps:
(1) pulverize: choose top grade Ganoderma, cut into slices, after pulverizing, also cross 100 mesh sieves;
(2) reduction treatment: take Ganoderma powder that 200g step (1) obtains and be added to reduction treatment 1h in 1% ascorbic acid solution of 1000ml and namely obtain reduction Ganoderma mixture;
(3) freeze thawing: reduction Ganoderma mixture step (2) handled well is placed in freeze thawing case, adds liquid nitrogen multigelation 6 times;
(4) breaking cellular wall: use the reduction Ganoderma mixture of 40% alcoholic solution to step (3) freeze thawing treatment to carry out ultrasonic air alveolation breaking cellular wall, the supersonic frequency of ultrasonic output 440W, employing 60kHz, supersound process 30min, stagnate 8min, supersound process 32min again, concentrated ultrasonic liquid obtains breaking cellular wall and concentrates lucidum liquid;
(5) supercritical CO
2extraction: get breaking cellular wall that step (4) obtains and concentrate lucidum liquid and carry out supercritical CO
2extraction, extraction conditions is pressure 14MPa, temperature 32 DEG C, dynamic extraction time 110min, CO
2flow 1mL/min, counterbalance valve temperature 45 C, collects extract classification;
(6) lyophilization.
Embodiment 3: a kind of high concentration Ganoderma triterpenoids and triterpene saponin composite extracting method, comprise the steps:
(1) pulverize: choose top grade Ganoderma, cut into slices, after pulverizing, also cross 100 mesh sieves;
(2) reduction treatment: take Ganoderma powder that 400g step (1) obtains and be added to reduction treatment 1.5h in 1% ascorbic acid solution of 1200ml and namely obtain reduction Ganoderma mixture;
(3) freeze thawing: reduction Ganoderma mixture step (2) handled well is placed in freeze thawing case, adds liquid nitrogen multigelation 7 times;
(4) breaking cellular wall: use the reduction Ganoderma mixture of 40% alcoholic solution to step (3) freeze thawing treatment to carry out ultrasonic air alveolation breaking cellular wall, the supersonic frequency of ultrasonic output 420W, employing 55kHz, supersound process 30min, stagnate 12min, supersound process 32min again, concentrated ultrasonic liquid obtains breaking cellular wall and concentrates lucidum liquid;
(5) supercritical CO
2extraction: get breaking cellular wall that step (4) obtains and concentrate lucidum liquid and carry out supercritical CO
2extraction, extraction conditions is pressure 14MPa, temperature 30 DEG C, dynamic extraction time 105min, CO
2flow 1mL/min, counterbalance valve temperature 45 C, collects extract classification;
(6) lyophilization.
The above; be only the specific embodiment of the present invention; but protection scope of the present invention is not limited thereto; any those of ordinary skill in the art are in the technical scope disclosed by the present invention; the change can expected without creative work or replacement, all should be encompassed within protection scope of the present invention.
Claims (1)
1. high concentration Ganoderma triterpenoids and a triterpene saponin composite extracting method, is characterized in that comprising the steps:
(1) pulverize: choose top grade Ganoderma, cut into slices, after pulverizing, also cross 100 mesh sieves;
(2) reduction treatment: the Ganoderma powder that step (1) obtains is added reduction treatment 1-2h in 1% ascorbic acid solution and namely obtain reduction Ganoderma mixture, the ratio of described Ganoderma powder and 1% ascorbic acid solution is m:v is 1:3-5;
(3) freeze thawing: reduction Ganoderma mixture step (2) handled well is placed in freeze thawing case, adds liquid nitrogen multigelation 6-8 time;
(4) breaking cellular wall: use the reduction Ganoderma mixture of 40% alcoholic solution to step (3) freeze thawing treatment to carry out ultrasonic air alveolation breaking cellular wall, the supersonic frequency of ultrasonic output 400-440W, employing 50-60kHz, supersound process 30-45min, stagnate 8-12min, supersound process 28-32min again, concentrated ultrasonic liquid obtains breaking cellular wall and concentrates lucidum liquid;
(5) supercritical CO
2extraction: get breaking cellular wall that step (4) obtains and concentrate lucidum liquid and carry out supercritical CO
2extraction, extraction conditions is, pressure 14MPa, temperature 30-32 DEG C, dynamic extraction time 100-110min, CO
2flow 1mL/min, counterbalance valve temperature 45 C, collects extract classification;
(6) lyophilization.
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Cited By (6)
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| CN105902578A (en) * | 2016-04-27 | 2016-08-31 | 杭州海王生物工程有限公司 | Extraction method of triterpenoid in Ganoderma lucidum spore |
| CN108653343A (en) * | 2018-07-27 | 2018-10-16 | 萃博士（平潭）生物科技有限公司 | It is a kind of for anticancer, liver protection Antrodia camphorata extract preparation method |
| CN108968031A (en) * | 2018-08-06 | 2018-12-11 | 深圳市玺越生物科技有限公司 | The antitumor row liver poison Wild ganoderma product of anticancer and technology of preparing |
| CN109097233A (en) * | 2018-07-30 | 2018-12-28 | 福州迈康医药科技有限公司 | A kind of Antrodia camphorata health liquor and its concocting method |
| WO2020186747A1 (en) * | 2019-03-21 | 2020-09-24 | 李和伟 | Freeze-dried formulation, preparation method and application thereof |
| CN112138031A (en) * | 2020-09-08 | 2020-12-29 | 广东都市菜族农业科技有限公司 | Preparation method and application of ganoderma lucidum spore powder extract containing ganoderma lucidum triterpene and ganoderma lucidum polysaccharide |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105902578A (en) * | 2016-04-27 | 2016-08-31 | 杭州海王生物工程有限公司 | Extraction method of triterpenoid in Ganoderma lucidum spore |
| CN105902578B (en) * | 2016-04-27 | 2019-05-10 | 杭州海王生物工程有限公司 | The extracting method of triterpene compound in a kind of lucidum spore powder |
| CN108653343A (en) * | 2018-07-27 | 2018-10-16 | 萃博士（平潭）生物科技有限公司 | It is a kind of for anticancer, liver protection Antrodia camphorata extract preparation method |
| CN109097233A (en) * | 2018-07-30 | 2018-12-28 | 福州迈康医药科技有限公司 | A kind of Antrodia camphorata health liquor and its concocting method |
| CN108968031A (en) * | 2018-08-06 | 2018-12-11 | 深圳市玺越生物科技有限公司 | The antitumor row liver poison Wild ganoderma product of anticancer and technology of preparing |
| WO2020186747A1 (en) * | 2019-03-21 | 2020-09-24 | 李和伟 | Freeze-dried formulation, preparation method and application thereof |
| CN112138031A (en) * | 2020-09-08 | 2020-12-29 | 广东都市菜族农业科技有限公司 | Preparation method and application of ganoderma lucidum spore powder extract containing ganoderma lucidum triterpene and ganoderma lucidum polysaccharide |
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