CN105902578A - Extraction method of triterpenoid in Ganoderma lucidum spore - Google Patents
Extraction method of triterpenoid in Ganoderma lucidum spore Download PDFInfo
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- CN105902578A CN105902578A CN201610268953.5A CN201610268953A CN105902578A CN 105902578 A CN105902578 A CN 105902578A CN 201610268953 A CN201610268953 A CN 201610268953A CN 105902578 A CN105902578 A CN 105902578A
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- 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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- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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- A61K2236/30—Extraction of the material
- A61K2236/35—Extraction with lipophilic solvents, e.g. Hexane or petrol ether
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- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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Abstract
The invention relates to the technical field of fungus treatment, in particular to an extraction method of triterpenoid in Ganoderma lucidum spore. The extraction method is performed by means of wall breaking first and extracting second, and extract obtained from Ganoderma lucidum spore is mainly triterpenoid. The extraction method is low in technical difficulty, and active ingredients of Ganoderma lucidum spore easier for human body to absorb can be obtained, so that utilization rate of Ganoderma lucidum spore is increased.
Description
Technical field
The present invention relates to mushroom processing technology field, be specifically related to the extracting method of triterpenoid compound in a kind of Ganoderma spore powder.
Background technology
Ganoderma spore is the sexual reproductive cell of Ganoderma, containing whole genetic activities materials of Ganoderma, has the effect such as antitumor, blood sugar lowering and immunomodulating, in pharmacology with there is application clinically, is also a kind of good natural health-care products raw material.Ganoderma spore contains the antitumorigenic substances such as abundant polysaccharide, triterpenoid compound, polypeptide, nucleic acid, organic germanium, and ganoderma lucidum triterpene compounds is antineoplastic main functional component.Ganoderma lucidum triterpene compounds is present in Ganoderma spore oil, has physiology and pharmacologically active widely, and its exploitation has wide market prospect with application.
Ganoderma spore powder be Ganoderma in the growth and maturity phase, the most small avette sexual cell shot out of being hit by a bullet from Ganoderma lamella, i.e. the seed of Ganoderma, it has condensed the elite of Ganoderma, has had whole hereditary materials and the health-care effect of Ganoderma.But Ganoderma spore wall has two-layer, internal containing 1-2 oil droplet, outer wall is made up of one layer of hard chitin mass shell, insoluble fibre and cellulose, there is the strongest resistance to acids and bases, prevent solvent that the extraction of Ganoderma spore oil is processed, only opening this double wall shell, its effective ingredient just can be immediately used by the body absorption.Scientific experiments confirms, taking the spore of non-breaking cellular wall, the effective ingredient of only 10%～20% can be absorbed by the body, and after breaking cellular wall, effective ingredient absorbance is more than 90%.
Ganoderma lucidum triterpene compounds is present in Ganoderma spore oil, is the main functional component of Ganoderma spore, breaking trachytectum of glossy ganoderma be Ganoderma spore Related product must be through operation.Extracting method many employings acid-base method of Ganoderma spore oil at present, enzyme process, defect is that wall breaking rate of ganoderma lucidum spores is low, and Ganoderma spore oil yield is low, the most also can destroy the effective ingredient of Ganoderma spore oil；Additionally, also microwave method, supercritical ultrasonics technology, liquid nitrogen quenching method, although these methods can improve Ganoderma spore oil yield, but working (machining) efficiency is low, and cost is high, is only applicable to laboratory operation, it is difficult to realize industrialized production.Although having multiple technologies at present can complete the broken wall treatment to Ganoderma spore powder, but the triterpenes Ganodenic acid unstable chemcial property contained by Ganoderma spore powder, while completing breaking cellular wall, how to ensure that effective component of glossy ganoderma is not destroyed during breaking cellular wall to greatest extent, and complete after breaking cellular wall again can stable existence, be the most still a technical barrier not having to solve.It is therefore desirable to extract triterpenoid compound to improve its utilization rate.
Summary of the invention
The invention aims to solve the problems referred to above, it is provided that the extracting method of triterpenoid compound in a kind of Ganoderma spore powder.
Here final products are the extract of Ganoderma spore powder, and are mainly composed of the mixture of triterpenoid compound.
In order to reach foregoing invention purpose, the present invention by the following technical solutions:
The extracting method of triterpenoid compound in a kind of Ganoderma spore powder, comprises the following steps:
(1) first Ganoderma spore powder is put in the sodium hydroxide solution that mass concentration is 0.05-0.15%, ultrasonic immersion 1-3h；Then add water and chitinolytic enzyme after filtering, decompose 1-2h, be dried at 35-50 DEG C after filtration；Drying time is at 5-10h；Ultrasonic power is 0.8-1.5w/cm2, frequency is 35-40KHz；
(2) dried Ganoderma spore powder employing supersonic jet mill is pulverized at-10 DEG C to-5 DEG C；
(3) addition Ganoderma spore powder is joined in microwave reflux extracting device, add in water and mixed liquor that butanol proportioning is 3:1 and extract 2-4 time, vacuum filtration；Petroleum ether microwave counter current is used to extract 1-3 time filtering residue the most again；
(4) in two kinds of filtrate, add trehalose, after stirring, all use macroporous adsorbent resin to adsorb；Add trehalose and can promote the adsorbent resin absorption to effective ingredient；Add trehalose and improve the rate of adsorption.
(5) then use concentration expressed in percentage by volume for 8-10 column volume of 60-70% ethanol elution, collecting 60-70% ethanol elution, concentrating under reduced pressure, reclaim ethanol, drying under reduced pressure, obtain triterpenoid compound.
As preferably, in step (1), the ultrasonic Ganoderma spore powder soaked after filtering is added to the water, and in Ganoderma spore powder, the addition of chitinolytic enzyme is 3000-4000u/g, adds ascorbic acid 3-5g in the most every 1kg Ganoderma spore powder.
Ascorbic acid controls the activity of enzyme, it is to avoid enzyme, by the chitin excessive decomposition of spore powder outer wall, causes loss.
As preferably, the ethanol water kind in step (5) is additionally added the glycine betaine that mass percent is 0.05-0.1%.
Add glycine betaine and can accelerate the extract i.e. abjection of triterpenoid compound.
As preferably, in step (1), the consumption of sodium hydroxide solution is every gram of Ganoderma spore powder 10ml.
As preferably, the extraction time that in step (3), each microwave counter current extracts is 10-15min.
The present invention compared with prior art, provides the benefit that:
1 method and technology difficulty is relatively low；2 can obtain the effective component of ganoderma lucidum spore powder being easier to be absorbed by the body, thus improve the utilization rate of Ganoderma spore powder.
Detailed description of the invention
Below by specific embodiment, technical scheme is further described explanation.
If without specified otherwise, the raw material employed in embodiments of the invention is raw material commonly used in the art, and the method employed in embodiment is the conventional method of this area.
The extracting method of triterpenoid compound in a kind of Ganoderma spore powder, comprises the following steps:
(1) first Ganoderma spore powder is put in the sodium hydroxide solution that mass concentration is 0.05-0.15%, ultrasonic immersion 1-3h；Then add water and chitinolytic enzyme after filtering, decompose 1-2h, be dried at 35-50 DEG C after filtration；Drying time is at 5-10h；Ultrasonic power is 0.8-1.5w/cm2, frequency is 35-40KHz；The consumption of sodium hydroxide solution is every gram of Ganoderma spore powder 10ml, and in Ganoderma spore powder, the addition of chitinolytic enzyme is 3000-4000u/g, adds ascorbic acid 3-5g in the most every 1kg Ganoderma spore powder,
(2) dried Ganoderma spore powder employing supersonic jet mill is pulverized at-10 DEG C to-5 DEG C；
(3) addition Ganoderma spore powder is joined in microwave reflux extracting device, add in water and mixed liquor that butanol proportioning is 3:1 and extract 2-4 time, vacuum filtration；Petroleum ether microwave counter current is used to extract 1-3 time filtering residue the most again；The extraction time that microwave counter current extracts every time is 10-15min；
(4) in two kinds of filtrate, add trehalose, after stirring, all use macroporous adsorbent resin to adsorb；
(5) then using concentration expressed in percentage by volume for using 8-10 column volume of 60-70% ethanol elution, ethanol water kind is additionally added the glycine betaine that mass percent is 0.05-0.1%, collects 60-70% ethanol elution, concentrating under reduced pressure, reclaim ethanol, drying under reduced pressure, obtain triterpenoid compound.
Embodiment
1
:
The extracting method of triterpenoid compound in a kind of Ganoderma spore powder, comprises the following steps:
(1) first Ganoderma spore powder is put in the sodium hydroxide solution that mass concentration is 0.05%, ultrasonic immersion 3h；Then adding water and chitinolytic enzyme after filtering, in Ganoderma spore powder, the addition of chitinolytic enzyme is 3000u/g, adds ascorbic acid 5g, decomposes 1h, be dried after filtration at 50 DEG C in the most every 1kg Ganoderma spore powder；Drying time is at 5h；Ultrasonic power is 1.5w/cm2, frequency is 35KHz；The consumption of sodium hydroxide solution is every gram of Ganoderma spore powder 10ml；
(2) dried Ganoderma spore powder employing supersonic jet mill is pulverized at-5 DEG C；
(3) addition Ganoderma spore powder is joined in microwave reflux extracting device, add in water and mixed liquor that butanol proportioning is 3:1 and extract 2 times, vacuum filtration；Petroleum ether microwave counter current is used to extract 3 times filtering residue the most again；The extraction time that microwave counter current extracts every time is 10-15min
(4) in two kinds of filtrate, add trehalose, after stirring, all use macroporous adsorbent resin to adsorb；
(5) then use concentration expressed in percentage by volume for 8-10 column volume of 60-70% ethanol elution, collecting 60-70% ethanol elution, concentrating under reduced pressure, reclaim ethanol, drying under reduced pressure, obtain triterpenoid compound.
Embodiment
2
:
The extracting method of triterpenoid compound in a kind of Ganoderma spore powder, comprises the following steps:
(1) first Ganoderma spore powder is put in the sodium hydroxide solution that mass concentration is 0.15%, ultrasonic immersion 1h；Then adding water and chitinolytic enzyme after filtering, in Ganoderma spore powder, the addition of chitinolytic enzyme is 4000u/g, adds ascorbic acid 3g, decomposes 2h, be dried after filtration at 35 DEG C in the most every 1kg Ganoderma spore powder；Drying time is at 10h；Ultrasonic power is 0.8w/cm2, frequency is 40KHz；The consumption of sodium hydroxide solution is every gram of Ganoderma spore powder 10ml；
(2) dried Ganoderma spore powder employing supersonic jet mill is pulverized at-10 DEG C；
(3) addition Ganoderma spore powder is joined in microwave reflux extracting device, add in water and mixed liquor that butanol proportioning is 3:1 and extract 2-4 time, vacuum filtration；Petroleum ether microwave counter current is used to extract 1-3 time filtering residue the most again；The extraction time that microwave counter current extracts every time is 10-15min
(4) in two kinds of filtrate, add trehalose, after stirring, all use macroporous adsorbent resin to adsorb；
(5) then use concentration expressed in percentage by volume for 8-10 column volume of 60-70% ethanol elution, collecting 60-70% ethanol elution, concentrating under reduced pressure, reclaim ethanol, drying under reduced pressure, obtain triterpenoid compound.
Embodiment
3
:
The extracting method of triterpenoid compound in a kind of Ganoderma spore powder, comprises the following steps:
(1) first Ganoderma spore powder is put in the sodium hydroxide solution that mass concentration is 0.05%, ultrasonic immersion 3h；Then adding water and chitinolytic enzyme after filtering, decompose 1h, in Ganoderma spore powder, the addition of chitinolytic enzyme is 4000u/g, adds ascorbic acid 3g in the most every 1kg Ganoderma spore powder；It is dried at 50 DEG C after filtration；Drying time is at 5h；Ultrasonic power is 1.5w/cm2, frequency is 35KHz；The consumption of sodium hydroxide solution is every gram of Ganoderma spore powder 10ml；
(2) dried Ganoderma spore powder employing supersonic jet mill is pulverized at-5 DEG C；
(3) addition Ganoderma spore powder is joined in microwave reflux extracting device, add in water and mixed liquor that butanol proportioning is 3:1 and extract 2-4 time, vacuum filtration；Petroleum ether microwave counter current is used to extract 1-3 time filtering residue the most again；The extraction time that microwave counter current extracts every time is 10-15min；
(4) in two kinds of filtrate, add trehalose, after stirring, all use macroporous adsorbent resin to adsorb；
(5) then using concentration expressed in percentage by volume for using 8-10 column volume of 60-70% ethanol elution, ethanol water kind is additionally added the glycine betaine that mass percent is 0.05%, collects 60-70% ethanol elution, concentrating under reduced pressure, reclaim ethanol, drying under reduced pressure, obtain triterpenoid compound.
Embodiment
4
:
The extracting method of triterpenoid compound in a kind of Ganoderma spore powder, comprises the following steps:
(1) first Ganoderma spore powder is put in the sodium hydroxide solution that mass concentration is 0.15%, ultrasonic immersion 1h；Then adding water and chitinolytic enzyme after filtering, decompose 2h, in Ganoderma spore powder, the addition of chitinolytic enzyme is 3000u/g, adds ascorbic acid 5g in the most every 1kg Ganoderma spore powder；It is dried at 35 DEG C after filtration；Drying time is at 10h；Ultrasonic power is 0.8w/cm2, frequency is 40KHz；The consumption of sodium hydroxide solution is every gram of Ganoderma spore powder 10ml；
(2) dried Ganoderma spore powder employing supersonic jet mill is pulverized at-10 DEG C；
(3) addition Ganoderma spore powder is joined in microwave reflux extracting device, add in water and mixed liquor that butanol proportioning is 3:1 and extract 2-4 time, vacuum filtration；Petroleum ether microwave counter current is used to extract 1-3 time filtering residue the most again；The extraction time that microwave counter current extracts every time is 10-15min；
(4) in two kinds of filtrate, add trehalose, after stirring, all use macroporous adsorbent resin to adsorb；
(5) then using concentration expressed in percentage by volume for using 8-10 column volume of 60-70% ethanol elution, ethanol water kind is additionally added the glycine betaine that mass percent is 0.1%, collects 60-70% ethanol elution, concentrating under reduced pressure, reclaim ethanol, drying under reduced pressure, obtain triterpenoid compound.
Step (1) adds ascorbic acid than the yield rate being not added with improving 3-5%；Fast speed 3-7% can be added after step (5) adds glycine betaine.
Claims (5)
1. the extracting method of triterpenoid compound in a Ganoderma spore powder, it is characterised in that comprise the following steps:
(1) first Ganoderma spore powder is put in the sodium hydroxide solution that mass concentration is 0.05-0.15%, ultrasonic immersion 1-3h；Then add water and chitinolytic enzyme after filtering, decompose 1-2h, be dried at 35-50 DEG C after filtration；Drying time is at 5-10h；Ultrasonic power is 0.8-1.5w/cm2, frequency is 35-40KHz；
(2) dried Ganoderma spore powder employing supersonic jet mill is pulverized at-10 DEG C to-5 DEG C；
(3) addition Ganoderma spore powder is joined in microwave reflux extracting device, add in water and mixed liquor that butanol proportioning is 3:1 and extract 2-4 time, vacuum filtration；Petroleum ether microwave counter current is used to extract 1-3 time filtering residue the most again；
(4) in two kinds of filtrate, add trehalose, after stirring, all use macroporous adsorbent resin to adsorb；
(5) then use concentration expressed in percentage by volume for 8-10 column volume of 60-70% ethanol elution, collecting 60-70% ethanol elution, concentrating under reduced pressure, reclaim ethanol, drying under reduced pressure, obtain triterpenoid compound.
The extracting method of triterpenoid compound in a kind of Ganoderma spore powder the most according to claim 1, it is characterized in that, in step (1), the ultrasonic Ganoderma spore powder soaked after filtering is added to the water, in Ganoderma spore powder, the addition of chitinolytic enzyme is 3000-4000u/g, adds ascorbic acid 3-5g in the most every 1kg Ganoderma spore powder.
The extracting method of triterpenoid compound in a kind of Ganoderma spore powder the most according to claim 1, it is characterised in that the ethanol water kind in step (5) is additionally added the glycine betaine that mass percent is 0.05-0.1%.
The extracting method of triterpenoid compound in a kind of Ganoderma spore powder the most according to claim 1, it is characterised in that in step (1), the consumption of sodium hydroxide solution is every gram of Ganoderma spore powder 10ml.
The extracting method of triterpenoid compound in a kind of Ganoderma spore powder the most according to claim 1, it is characterised in that the extraction time that in step (3), each microwave counter current extracts is 10-15min.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106722875A (en) * | 2016-12-07 | 2017-05-31 | 盐城工学院 | The extracting method and Ganoderma lucidum of a kind of ganodenic acid |
| CN109893547A (en) * | 2019-02-22 | 2019-06-18 | 湖州柳荫生物科技有限公司 | A method of extracting ganodenic acid and ganoderma lucidum polysaccharide from ganoderma lucidum |
| CN111437320A (en) * | 2020-05-18 | 2020-07-24 | 德化县仙铭生态农林有限公司 | Efficient bacteriostatic ganoderma lucidum triterpene tea oil capsule and preparation process 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 |
| CN113024682A (en) * | 2021-03-16 | 2021-06-25 | 贵州高山生物科技有限公司 | Method for extracting ganoderma lucidum spore powder polysaccharide |
| CN114618689A (en) * | 2022-05-16 | 2022-06-14 | 广东华夏友美生物科技有限公司 | Ganoderma triterpene extraction and separation equipment and extraction and separation process thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106722875A (en) * | 2016-12-07 | 2017-05-31 | 盐城工学院 | The extracting method and Ganoderma lucidum of a kind of ganodenic acid |
| CN109893547A (en) * | 2019-02-22 | 2019-06-18 | 湖州柳荫生物科技有限公司 | A method of extracting ganodenic acid and ganoderma lucidum polysaccharide from ganoderma lucidum |
| CN109893547B (en) * | 2019-02-22 | 2021-08-20 | 湖州柳荫生物科技有限公司 | Method for extracting ganoderma triterpene and ganoderma polysaccharide from ganoderma |
| CN111437320A (en) * | 2020-05-18 | 2020-07-24 | 德化县仙铭生态农林有限公司 | Efficient bacteriostatic ganoderma lucidum triterpene tea oil capsule and preparation process 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 |
| CN113024682A (en) * | 2021-03-16 | 2021-06-25 | 贵州高山生物科技有限公司 | Method for extracting ganoderma lucidum spore powder polysaccharide |
| CN114618689A (en) * | 2022-05-16 | 2022-06-14 | 广东华夏友美生物科技有限公司 | Ganoderma triterpene extraction and separation equipment and extraction and separation process thereof |
| CN114618689B (en) * | 2022-05-16 | 2022-08-12 | 广东华夏友美生物科技有限公司 | Ganoderma triterpene extraction and separation equipment and extraction and separation process thereof |
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