CN105902578B - The extracting method of triterpene compound in a kind of lucidum spore powder - Google Patents
The extracting method of triterpene compound in a kind of lucidum spore powder Download PDFInfo
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- CN105902578B CN105902578B CN201610268953.5A CN201610268953A CN105902578B CN 105902578 B CN105902578 B CN 105902578B CN 201610268953 A CN201610268953 A CN 201610268953A CN 105902578 B CN105902578 B CN 105902578B
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- 239000000843 powder Substances 0.000 title claims abstract description 70
- -1 triterpene compound Chemical class 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000000284 extract Substances 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 49
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- 235000019441 ethanol Nutrition 0.000 claims description 21
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 18
- 102000004190 Enzymes Human genes 0.000 claims description 17
- 108090000790 Enzymes Proteins 0.000 claims description 17
- 238000002604 ultrasonography Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 14
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 238000000605 extraction Methods 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 14
- 230000001794 chitinolytic effect Effects 0.000 claims description 13
- HDTRYLNUVZCQOY-UHFFFAOYSA-N α-D-glucopyranosyl-α-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OC1C(O)C(O)C(O)C(CO)O1 HDTRYLNUVZCQOY-UHFFFAOYSA-N 0.000 claims description 9
- HDTRYLNUVZCQOY-WSWWMNSNSA-N Trehalose Natural products O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 HDTRYLNUVZCQOY-WSWWMNSNSA-N 0.000 claims description 9
- HDTRYLNUVZCQOY-LIZSDCNHSA-N alpha,alpha-trehalose Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 HDTRYLNUVZCQOY-LIZSDCNHSA-N 0.000 claims description 9
- 229960005070 ascorbic acid Drugs 0.000 claims description 9
- 235000010323 ascorbic acid Nutrition 0.000 claims description 9
- 239000011668 ascorbic acid Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 239000011347 resin Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 8
- 230000002745 absorbent Effects 0.000 claims description 7
- 239000002250 absorbent Substances 0.000 claims description 7
- 239000000654 additive Substances 0.000 claims description 7
- 230000000996 additive effect Effects 0.000 claims description 7
- 229960003237 betaine Drugs 0.000 claims description 7
- 238000010828 elution Methods 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 7
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical compound C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000003208 petroleum Substances 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 5
- 238000007654 immersion Methods 0.000 claims description 2
- 240000008397 Ganoderma lucidum Species 0.000 abstract description 26
- 235000001637 Ganoderma lucidum Nutrition 0.000 abstract description 26
- 238000005516 engineering process Methods 0.000 abstract description 5
- 235000001674 Agaricus brunnescens Nutrition 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229920002101 Chitin Polymers 0.000 description 2
- 241000222336 Ganoderma Species 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000000259 anti-tumor effect Effects 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 150000003648 triterpenes Chemical class 0.000 description 2
- RDMQPKIDHAFXKA-JNORPAGFSA-N Ganoderic Acid Am1 Chemical compound C([C@@]12C)C[C@H](O)C(C)(C)[C@@H]1CC(=O)C1=C2C(=O)C[C@]2(C)[C@@H]([C@@H](CC(=O)CC(C)C(O)=O)C)CC(=O)[C@]21C RDMQPKIDHAFXKA-JNORPAGFSA-N 0.000 description 1
- 229930182735 Ganoderic acid Natural products 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 244000000231 Sesamum indicum Species 0.000 description 1
- 235000003434 Sesamum indicum Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000002622 anti-tumorigenesis Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000001925 catabolic effect Effects 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002068 genetic effect Effects 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000001900 immune effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- AXONCVPTTFHNOI-UHFFFAOYSA-N kairine Chemical compound C1=CC(O)=C2N(C)CCCC2=C1 AXONCVPTTFHNOI-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 102000039446 nucleic acids Human genes 0.000 description 1
- 108020004707 nucleic acids Proteins 0.000 description 1
- 150000007523 nucleic acids Chemical class 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 230000035479 physiological effects, processes and functions Effects 0.000 description 1
- 229920001184 polypeptide Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 210000005132 reproductive cell Anatomy 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- 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
-
- 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
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
-
- 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
- A61K2236/30—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 or decoction
-
- 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
- A61K2236/30—Extraction of the material
- A61K2236/35—Extraction with lipophilic solvents, e.g. Hexane or petrol ether
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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
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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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
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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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
- A61K2236/55—Liquid-liquid separation; Phase separation
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- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Medicines Containing Plant Substances (AREA)
- Micro-Organisms Or Cultivation Processes Thereof (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The present invention relates to mushroom processing technology fields, more particularly to a kind of extracting method of triterpene compound in lucidum spore powder, what this method was carried out by the way of being extracted after first broken wall, the extract obtained by lucidum spore powder, predominantly triterpene compound, this method technical difficulty are lower;The effective component of ganoderma lucidum spore powder for being easier to be absorbed by the body can be obtained, to improve the utilization rate of lucidum spore powder.
Description
Technical field
The present invention relates to mushroom processing technology fields, and in particular to the extraction of triterpene compound in a kind of lucidum spore powder
Method.
Background technique
Reishi sporule is the sexual reproductive cell of ganoderma lucidum, whole genetic activities substances containing ganoderma lucidum, has antitumor, drop
, in pharmacology and clinically there are application and a kind of good natural health-care products raw material in the effects of blood glucose and immunological regulation.Spirit
The antitumorigenic substances such as Ganoderma lucidum spore polysaccharide rich in, triterpene compound, polypeptide, nucleic acid, organic germanium, and ganoderma lucidum triterpene
Closing object is antitumor main functional component.Ganoderma lucidum triterpene compounds are present in ganoderma lucidum spore oil, have extensive physiology
And pharmacological activity, its exploitation and application have a vast market foreground.
Lucidum spore powder is ganoderma lucidum in growth and maturity phase, the extremely small oval reproduction ejected from glossy ganoderma lamella
Cell, the i.e. seed of ganoderma lucidum, have agglomerated the essence of ganoderma lucidum, whole inhereditary materials and health-care effect with ganoderma lucidum.But it is clever
Ganoderma lucidum spore wall has two layers, and 1-2 oil droplet is contained in inside, and outer wall is by one layer of hard chitin mass shell, insoluble fibre and fiber
Element composition, there is very strong resistance to acid and alkali, prevents solvent to process the extraction of ganoderma lucidum spore oil, only opens this double wall shell,
Its effective component can just be immediately used by the body absorption.Scientific experiment confirms, take the spore of non-broken wall, and only 10%~20% has
Effect ingredient can be absorbed by the body, and effective component absorptivity is 90% or more after broken wall.
Ganoderma lucidum triterpene compounds are present in ganoderma lucidum spore oil, are the main functional components of Reishi sporule, and Reishi sporule is broken
Wall is the necessary process of Reishi sporule Related product.The extracting method of ganoderma lucidum spore oil mostly uses acid-base method, enzyme process, defect at present
It is that wall breaking rate of ganoderma lucidum spores is low, ganoderma lucidum spore oil yield is low, while can also destroy the effective component of ganoderma lucidum spore oil;In addition, also
There are microwave method, supercritical ultrasonics technology, liquid nitrogen quenching method, although these methods can improve ganoderma lucidum spore oil yield, processing efficiency is low,
It is at high cost, it is only applicable to laboratory operation, it is difficult to realize industrialized production.Although existing multiple technologies can be completed to spirit at present
The broken wall treatment of Ganoderma lucidum spore powder, but the triterpenes ganoderic acid unstable chemcial property as contained by lucidum spore powder, how
It completes to guarantee that effective component of glossy ganoderma is not destroyed during broken wall to the maximum extent while broken wall, and energy again after completion broken wall
It is stabilized, is still the technical problem not solved at present.It is therefore desirable to triterpene compound extract with
Improve its utilization rate.
Summary of the invention
The purpose of the present invention is to solve the above problem, a kind of extraction of triterpene compound in lucidum spore powder is provided
Method.
Here final products are the extract of lucidum spore powder, and main component is the mixture of triterpene compound.
In order to achieve the above object of the invention, the invention adopts the following technical scheme:
The extracting method of triterpene compound in a kind of lucidum spore powder, comprising the following steps:
(1) lucidum spore powder is put into the sodium hydroxide solution that mass concentration is 0.05-0.15% first, ultrasound is impregnated
1-3h;Then water and chitinolytic enzyme are added after filtering, decomposes 1-2h, it is dry at 35-50 DEG C after filtering;Drying time exists
5-10h;The power of ultrasound is 0.8-1.5w/cm2, frequency 35-40KHz;
(2) lucidum spore powder after drying is crushed at -10 DEG C to -5 DEG C using supersonic jet mill;
(3) lucidum spore powder will be added to be added in microwave reflux extracting device, water is added and butanol proportion is the mixed of 3:1
It closes and is extracted 2-4 times in liquid, is filtered by vacuum;Then filter residue is extracted 1-3 times using petroleum ether microwave counter current again;
(4) trehalose is added in two kinds of filtrates, after mixing evenly, is all made of macroporous absorbent resin and is adsorbed;It is added
Trehalose can promote to adsorb absorption of the resin to effective component;Trehalose is added and improves the rate of adsorption.
(5) then use concentration expressed in percentage by volume for 8-10 column volume of 60-70% ethanol elution, collection 60-70% second
Alcohol eluen is concentrated under reduced pressure, and recycles ethyl alcohol, is dried under reduced pressure, obtains triterpene compound.
Preferably, the filtered lucidum spore powder of ultrasound immersion is added to the water in step (1), it is several in lucidum spore powder
The additive amount of fourth matter catabolic enzyme is 3000-4000u/g, while ascorbic acid 3-5g being added in every 1kg lucidum spore powder.
Ascorbic acid controls the activity of enzyme, avoids chitin excessive decomposition of the enzyme by conidia powder outer wall, causes to be lost.
Preferably, the ethanol water kind in step (5) is additionally added the glycine betaine that mass percent is 0.05-0.1%.
Glycine betaine, which is added, can accelerate the extract i.e. abjection of triterpene compound.
Preferably, the dosage of sodium hydroxide solution is every gram of lucidum spore powder 10ml in step (1).
Preferably, the extraction time that each microwave counter current extracts in step (3) is 10-15min.
Compared with prior art, the present invention beneficial effect is:
1 method and technology difficulty is lower;2 can obtain the effective component of ganoderma lucidum spore powder for being easier to be absorbed by the body, thus
Improve the utilization rate of lucidum spore powder.
Specific embodiment
Below by specific embodiment the technical scheme of the present invention will be further described explanation.
If raw material employed in the embodiment of the present invention is raw material commonly used in the art without specified otherwise, implement
Method employed in example, is the conventional method of this field.
The extracting method of triterpene compound in a kind of lucidum spore powder, comprising the following steps:
(1) lucidum spore powder is put into the sodium hydroxide solution that mass concentration is 0.05-0.15% first, ultrasound is impregnated
1-3h;Then water and chitinolytic enzyme are added after filtering, decomposes 1-2h, it is dry at 35-50 DEG C after filtering;Drying time exists
5-10h;The power of ultrasound is 0.8-1.5w/cm2, frequency 35-40KHz;The dosage of sodium hydroxide solution is every kairine sesame spore
Sub- powder 10ml, the additive amount of chitinolytic enzyme is 3000-4000u/g in lucidum spore powder, while in every 1kg lucidum spore powder
Ascorbic acid 3-5g is added,
(2) lucidum spore powder after drying is crushed at -10 DEG C to -5 DEG C using supersonic jet mill;
(3) lucidum spore powder will be added to be added in microwave reflux extracting device, water is added and butanol proportion is the mixed of 3:1
It closes and is extracted 2-4 times in liquid, is filtered by vacuum;Then filter residue is extracted 1-3 times using petroleum ether microwave counter current again;Each microwave counter current
The extraction time of extraction is 10-15min;
(4) trehalose is added in two kinds of filtrates, after mixing evenly, is all made of macroporous absorbent resin and is adsorbed;
(5) then use concentration expressed in percentage by volume for 8-10 column volume of 60-70% ethanol elution, ethanol water kind is also
The glycine betaine that mass percent is 0.05-0.1% is added, collects 60-70% ethanol eluate, is concentrated under reduced pressure, recycles ethyl alcohol, subtracts
It press dry dry, obtains triterpene compound.
Embodiment 1:
The extracting method of triterpene compound in a kind of lucidum spore powder, comprising the following steps:
(1) lucidum spore powder is put into the sodium hydroxide solution that mass concentration is 0.05% first, ultrasound impregnates 3h;So
Water and chitinolytic enzyme are added after filtering afterwards, the additive amount of chitinolytic enzyme is 3000u/g in lucidum spore powder, while every
Ascorbic acid 5g is added in 1kg lucidum spore powder, decomposes 1h, it is dry at 50 DEG C after filtering;Drying time is in 5h;The function of ultrasound
Rate is 1.5w/cm2, frequency 35KHz;The dosage of sodium hydroxide solution is every gram of lucidum spore powder 10ml;
(2) lucidum spore powder after drying is crushed at -5 DEG C using supersonic jet mill;
(3) lucidum spore powder will be added to be added in microwave reflux extracting device, water is added and butanol proportion is the mixed of 3:1
It closes and is extracted 2 times in liquid, is filtered by vacuum;Then filter residue is extracted 3 times using petroleum ether microwave counter current again;Each microwave counter current extracts
Extraction time be 10-15min
(4) trehalose is added in two kinds of filtrates, after mixing evenly, is all made of macroporous absorbent resin and is adsorbed;
(5) then use concentration expressed in percentage by volume for 8-10 column volume of 60-70% ethanol elution, collection 60-70% second
Alcohol eluen is concentrated under reduced pressure, and recycles ethyl alcohol, is dried under reduced pressure, obtains triterpene compound.
Embodiment 2:
The extracting method of triterpene compound in a kind of lucidum spore powder, comprising the following steps:
(1) lucidum spore powder is put into the sodium hydroxide solution that mass concentration is 0.15% first, ultrasound impregnates 1h;So
Water and chitinolytic enzyme are added after filtering afterwards, the additive amount of chitinolytic enzyme is 4000u/g in lucidum spore powder, while every
Ascorbic acid 3g is added in 1kg lucidum spore powder, decomposes 2h, it is dry at 35 DEG C after filtering;Drying time is in 10h;Ultrasound
Power is 0.8w/cm2, frequency 40KHz;The dosage of sodium hydroxide solution is every gram of lucidum spore powder 10ml;
(2) lucidum spore powder after drying is crushed at -10 DEG C using supersonic jet mill;
(3) lucidum spore powder will be added to be added in microwave reflux extracting device, water is added and butanol proportion is the mixed of 3:1
It closes and is extracted 2-4 times in liquid, is filtered by vacuum;Then filter residue is extracted 1-3 times using petroleum ether microwave counter current again;Each microwave counter current
The extraction time of extraction is 10-15min
(4) trehalose is added in two kinds of filtrates, after mixing evenly, is all made of macroporous absorbent resin and is adsorbed;
(5) then use concentration expressed in percentage by volume for 8-10 column volume of 60-70% ethanol elution, collection 60-70% second
Alcohol eluen is concentrated under reduced pressure, and recycles ethyl alcohol, is dried under reduced pressure, obtains triterpene compound.
Embodiment 3:
The extracting method of triterpene compound in a kind of lucidum spore powder, comprising the following steps:
(1) lucidum spore powder is put into the sodium hydroxide solution that mass concentration is 0.05% first, ultrasound impregnates 3h;So
Water and chitinolytic enzyme are added after filtering afterwards, decomposes 1h, the additive amount of chitinolytic enzyme is 4000u/ in lucidum spore powder
G, while ascorbic acid 3g being added in every 1kg lucidum spore powder;It is dry at 50 DEG C after filtering;Drying time is in 5h;Ultrasound
Power is 1.5w/cm2, frequency 35KHz;The dosage of sodium hydroxide solution is every gram of lucidum spore powder 10ml;
(2) lucidum spore powder after drying is crushed at -5 DEG C using supersonic jet mill;
(3) lucidum spore powder will be added to be added in microwave reflux extracting device, water is added and butanol proportion is the mixed of 3:1
It closes and is extracted 2-4 times in liquid, is filtered by vacuum;Then filter residue is extracted 1-3 times using petroleum ether microwave counter current again;Each microwave counter current
The extraction time of extraction is 10-15min;
(4) trehalose is added in two kinds of filtrates, after mixing evenly, is all made of macroporous absorbent resin and is adsorbed;
(5) then use concentration expressed in percentage by volume for 8-10 column volume of 60-70% ethanol elution, ethanol water kind is also
The glycine betaine that mass percent is 0.05% is added, collects 60-70% ethanol eluate, is concentrated under reduced pressure, recycles ethyl alcohol, decompression is dry
It is dry, obtain triterpene compound.
Embodiment 4:
The extracting method of triterpene compound in a kind of lucidum spore powder, comprising the following steps:
(1) lucidum spore powder is put into the sodium hydroxide solution that mass concentration is 0.15% first, ultrasound impregnates 1h;So
Water and chitinolytic enzyme are added after filtering afterwards, decomposes 2h, the additive amount of chitinolytic enzyme is 3000u/ in lucidum spore powder
G, while ascorbic acid 5g being added in every 1kg lucidum spore powder;It is dry at 35 DEG C after filtering;Drying time is in 10h;Ultrasound
Power is 0.8w/cm2, frequency 40KHz;The dosage of sodium hydroxide solution is every gram of lucidum spore powder 10ml;
(2) lucidum spore powder after drying is crushed at -10 DEG C using supersonic jet mill;
(3) lucidum spore powder will be added to be added in microwave reflux extracting device, water is added and butanol proportion is the mixed of 3:1
It closes and is extracted 2-4 times in liquid, is filtered by vacuum;Then filter residue is extracted 1-3 times using petroleum ether microwave counter current again;Each microwave counter current
The extraction time of extraction is 10-15min;
(4) trehalose is added in two kinds of filtrates, after mixing evenly, is all made of macroporous absorbent resin and is adsorbed;
(5) then use concentration expressed in percentage by volume for 8-10 column volume of 60-70% ethanol elution, ethanol water kind is also
The glycine betaine that mass percent is 0.1% is added, collects 60-70% ethanol eluate, is concentrated under reduced pressure, recycles ethyl alcohol, decompression is dry
It is dry, obtain triterpene compound.
In step (1) plus ascorbic acid can be improved the yield rate of 3-5% than being not added;Energy after addition glycine betaine in step (5)
Accelerate speed 3-7%.
Claims (5)
1. the extracting method of triterpene compound in a kind of lucidum spore powder, which comprises the following steps:
(1) lucidum spore powder is put into the sodium hydroxide solution that mass concentration is 0.05-0.15% first, ultrasound impregnates 1-3h;
Then water and chitinolytic enzyme are added after filtering, decomposes 1-2h, it is dry at 35-50 DEG C after filtering;Drying time is in 5-
10h;The power density of ultrasound is 0.8-1.5w/cm2, frequency 35-40KHz;
(2) lucidum spore powder after drying is crushed at -10 DEG C to -5 DEG C using supersonic jet mill;
(3) lucidum spore powder is added in microwave reflux extracting device, water and butanol proportion is added to mention in the mixed liquor of 3:1
It takes 2-4 times, is filtered by vacuum;Then filter residue is extracted 1-3 times using petroleum ether microwave counter current again;
(4) trehalose is added in two kinds of filtrates, after mixing evenly, is all made of macroporous absorbent resin and is adsorbed;
(5) it then uses concentration expressed in percentage by volume for 8-10 column volume of ethanol elution of 60-70%, collects 60-70% ethyl alcohol and wash
De- liquid, is concentrated under reduced pressure, and recycles ethyl alcohol, is dried under reduced pressure, obtains triterpene compound.
2. the extracting method of triterpene compound in a kind of lucidum spore powder according to claim 1, which is characterized in that step
Suddenly the filtered lucidum spore powder of ultrasound immersion is added to the water in (1), the additive amount of chitinolytic enzyme in lucidum spore powder
For 3000-4000U/g, while ascorbic acid 3-5g being added in every 1kg lucidum spore powder.
3. the extracting method of triterpene compound in a kind of lucidum spore powder according to claim 1, which is characterized in that step
Suddenly the glycine betaine that mass percent is 0.05-0.1% is additionally added in the ethanol water in (5).
4. the extracting method of triterpene compound in a kind of lucidum spore powder according to claim 1, which is characterized in that step
Suddenly the dosage of sodium hydroxide solution is every gram of lucidum spore powder 10ml in (1).
5. the extracting method of triterpene compound in a kind of lucidum spore powder according to claim 1, which is characterized in that step
Suddenly the extraction time that each microwave counter current extracts in (3) is 10-15min.
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