CN105663178A - Method for extracting inonotus obliquus total triterpenes - Google Patents
Method for extracting inonotus obliquus total triterpenes Download PDFInfo
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- CN105663178A CN105663178A CN201610179537.8A CN201610179537A CN105663178A CN 105663178 A CN105663178 A CN 105663178A CN 201610179537 A CN201610179537 A CN 201610179537A CN 105663178 A CN105663178 A CN 105663178A
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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
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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
- A61K2236/10—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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- 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
- A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
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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
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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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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- 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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Abstract
The invention discloses a method for extracting inonotus obliquus total triterpenes. The method includes: preprocessing, wall breaking, ultrasonic treatment, vacuum concentration, and total triterpene absorption and purification. The method has the advantages that cell walls are completely broken through the wall breaking, ultrasonic is used to assist extraction, nutrition loss and severe effective component damage, caused by high temperature, of the raw material are avoided; the total triterpenes in inonotus obliquus cells are promoted to dissolve out fast; compared with a traditional total triterpene extraction method, the method is low in energy consumption, high in total triterpene extraction rate and low in production cost; by the method combining the wall breaking and the ultrasonic extraction, the extraction rate of the inonotus obliquus total triterpenes is 1.15-1.72 times of that of the traditional extraction method.
Description
Technical field
The present invention relates to the edible mushrooms extracting method of a kind of enrichment mineral element, it is specifically related to the fine pore fungi total triterpene extracting method of a kind of birch.
Background technology
The fine pore fungi (Inonotusobliquus (Ach.exPers.) Pil á t) of birch also claims Phaeopoms obliquus, Chaga, belong to Basidiomycotina, Hymenomycetes, Aphyllophorales, Hymenochaetaceae, in foreign language datum, it often occurs with formal name used at school Inonotusobliquus. The fine pore fungi sclerotium of birch is warty, without handle, and surface black gray expandable, inner yellowish-brown, old rear surface drastic crack, hard, more crisp time dry. Have and strengthen immunity, the curative effects such as the prevention sick urine of sugar. As a kind of main active ingredient of the fine pore fungi of birch, three terpenes can be used for the prevention and therapy of diabetes, malignant tumour, cardiovascular disorder, hepatopathy and acquired immune deficiency syndrome (AIDS). In triterpene compound, trochol and derivative thereof have anti-treating leukemia, the special efficacies such as anti-hiv activity and anti-melanocyte tumor activity. Therefore, the fine pore fungi of birch has great pharmacy value. Mineral element is the important component part of humans and animals body, has important physiological function. The mineral element major part of enrichment in edible mushrooms exists with organic, and good stability, and wherein the mineral element of major part organic is all combined with the biomacromolecule such as protein, polysaccharide, and facilitates absorption and the utilization of mineral element. At present to the still few report of nutrition assay after the fine pore fungi triterpenoid extraction process of birch and enrichment mineral element, traditional triterpenes components extracting method: extraction process, semi-bionic extraction, chemical derivatization, ultrasonic circulation techniques etc. easily cause three terpene degradeds, supercritical fluid extraction becomes a kind of new extraction and separation technology in recent years, has the advantages such as composition activity and no solvent residue of remaining valid. But equipment is complicated, running cost height, extracts scope narrow, is not thus widely used.
Summary of the invention
The present invention is directed in above-mentioned technology the deficiency existed, it is provided that the fine pore fungi total triterpene extracting method of a kind of birch, solves energy consumption when extracting in prior art big, production cost height, the problem that extraction yield is low.
The technical solution used in the present invention is as follows:
An extracting method for the fine pore fungi total triterpene of birch, its concrete operation steps is as follows:
Step 1, pre-treatment: the fine pore fungi mycelia of birch under 60-80 DEG C of condition, dry 10-16 hour;
Step 2, broken wall: pulverized by fine for above-mentioned pretreated birch pore fungi mycelia broken wall, cross 200 order sieves, add 95% ethanol, and the mass ratio of 95% ethanol and mycelia is 30-50:1, is mixed with suspension, soaks 24h;
Step 3, ultrasonication: by fine for above-mentioned birch pore fungi suspension ultrasonication, 60-80 DEG C, power 400W, time 10-20min;
Step 4, concentrating under reduced pressure: the suspension after above-mentioned ultrasonication is evaporated to AmL, obtain AmL concentrated solution; Under 13000-16000r/min, 0-5 DEG C of condition, centrifugal 8-15min, gets supernatant liquor, adds 95% ethanol and be settled to AmL in supernatant liquor;
The absorption of step 5, total triterpene and purifying: with the flow velocity of 2BV/h, the liquid after above-mentioned fixed appearance being crossed macroporous adsorbent resin column chromatography, with 80% ethanol elution, collects the solution eluted after variable color, the solution eluted is extracting substance.
It is an advantage of the current invention that: the present invention takes broken wall to pulverize a kind of wall-breaking method hocketed with ultrasonic-assisted extraction, impels the high temperature that simultaneously avoids that cell breaks completely that raw material being said, the nutritive loss caused, effective constituent destroy serious detrimentally affect. The fine pore fungi total triterpene of ultrasonic-assisted extraction birch, mechanical effect also accelerates the fragmentation of cell walls, promotes the Fast Stripping of total triterpene active substance in born of the same parents. Compared with tradition Polyose extraction, broken wall pulverize and and ultrasonic-assisted extraction effectively combine, have that energy consumption is low, total triterpene extraction yield height, the feature that production cost is low. By broken wall combining ultrasonic ripple extracting method of the present invention, the fine pore fungi total triterpene extraction yield of birch is 1.15～1.72 times of traditional extraction process.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that the present invention extracts the fine pore fungi total triterpene of birch.
Embodiment
Embodiment 1
Step 1, pre-treatment: the fine pore fungi mycelia of birch under 70 DEG C of conditions, dry 12 hours;
Step 2, broken wall: pulverized by fine for above-mentioned pretreated birch pore fungi mycelia broken wall, cross 200 orders sieves, and taking that the fine pore fungi powder of 100g birch be dissolved in 100mL95% ethanol to be mixed with concentration is 2% suspension, soaks 24h;
Step 3, ultrasonication: by fine for above-mentioned birch pore fungi suspension ultrasonication, 70 DEG C, power 400W, time 15min;
Step 4, concentrating under reduced pressure: by the suspension after above-mentioned ultrasonication, under normal pressure 80 DEG C of conditions, be evaporated to 20mL, obtain concentrated solution; In 14000r/min, centrifugal 10min under 0 DEG C of condition, gets supernatant liquor, adds 95% ethanol and be settled to 20mL in supernatant liquor;
The absorption of step 5, total triterpene and purifying: be 1.5cm to diameter, the macroporous adsorptive resins that post length is 50cm carries out pre-treatment, with 95% alcohol immersion 24h, when the volume ratio being washed till effluent liquid and water with 95% ethanol again is 1:5 not muddy, wash with water afterwards to without alcohol taste, finally it is washed to neutrality, liquid after fixed for above-mentioned steps 4 appearance is crossed above-mentioned pretreated macroporous adsorbent resin column chromatography with the flow velocity of 2BV/h, with 80% ethanol elution, collecting the solution eluted after variable color, the solution eluted is extracting substance.
The fine pore fungi total triterpene Different Extraction Method extraction yield determination test of birch is as follows:
1, materials and methods
The fine pore fungi powder of birch: Shenyang engineering college life engineering institute edible mushrooms laboratory
2, the fine pore fungi total triterpene extracting method of birch
Get 2g, the fine pore fungi powder of 200 order birch, with 100mL95% alcohol immersion 24h, adopt as follows respectively:
1), laser heating refluxing extraction (cable type extractor according): extract 4h;
2), ultrasonic extraction: ultrasonic 15min;
3), rotary distillation extract: rotary distillation desorb 1 time, extract 15min afterwards, add 100 DEG C of distilled water 20mL, decompressing inner ebullition 5min.
The extraction yield of 3.1 total triterpene measures
Adopt Vanillin one ice acetic acid method to measure, take Oleanolic Acid as standard substance, at the corresponding relation of 550nm wavelength place bioassay standard thing mass concentration and absorbancy, preparation standard curve.
3.1.1 total triterpene extraction yield %=(the fine pore fungi quality of total triterpene quality/birch) × 100%
4, measurement result
4.1 Oleanolic Acid typical curves obtain regression equation: y=0.5726x+0.0229, R2=0.9805, record various method according to regression equation and extract the fine pore fungi total triterpene extraction yield of birch such as table 1.
5. conclusion
As shown in Table 1, ultrasonic extraction and other two kinds of methods differ obviously, therefore can determine the fine pore fungi total triterpene of broken wall combining ultrasonic ripple extraction method the most applicable extraction birch. Owing to the main component of the fine pore fungi cell walls of birch is pectin and Mierocrystalline cellulose, simple physical disruption methods, it is difficult to all cell wallss are carried out fragmentation. It is one broken wall mode efficiently that broken wall is pulverized, cell wall breaking can be made comparatively thorough, auxiliary ultrasonic processing, utilize the cavatition of ultrasonic lane generation, the fragmentation of mechanical effect acceleration cell walls, impel the stripping of intracellular organic matter thus improve total triterpene extraction yield and gained birch fine pore fungi total triterpene relatively other extracting method high purities.
Embodiment 2
An extracting method for the fine pore fungi total triterpene of birch, its concrete operation steps is as follows:
Step 1, pre-treatment: the fine pore fungi mycelia of birch under 60 DEG C of conditions, dry 16 hours;
Step 2, broken wall: pulverized by fine for above-mentioned pretreated birch pore fungi mycelia broken wall, cross 200 order sieves, add 95% ethanol, and the mass ratio of 95% ethanol and mycelia is 30:1, is mixed with suspension, soaks 24h;
Step 3, ultrasonication: by fine for above-mentioned birch pore fungi suspension ultrasonication, 60 DEG C, power 400W, time 20min;
Step 4, concentrating under reduced pressure: the suspension after above-mentioned ultrasonication is evaporated to AmL, obtain AmL concentrated solution; In 13000r/min, centrifugal 15min under 0 DEG C of condition, gets supernatant liquor, adds 95% ethanol and be settled to AmL in supernatant liquor;
The absorption of step 5, total triterpene and purifying: with the flow velocity of 2BV/h, the liquid after above-mentioned fixed appearance being crossed macroporous adsorbent resin column chromatography, with 80% ethanol elution, collects the solution eluted after variable color, the solution eluted is extracting substance.
Embodiment 3
An extracting method for the fine pore fungi total triterpene of birch, its concrete operation steps is as follows:
Step 1, pre-treatment: the fine pore fungi mycelia of birch under 80 DEG C of conditions, dry 10 hours;
Step 2, broken wall: pulverized by fine for above-mentioned pretreated birch pore fungi mycelia broken wall, cross 200 order sieves, add 95% ethanol, and the mass ratio of 95% ethanol and mycelia is 50:1, is mixed with suspension, soaks 24h;
Step 3, ultrasonication: by fine for above-mentioned birch pore fungi suspension ultrasonication, 80 DEG C, power 400W, time 10min;
Step 4, concentrating under reduced pressure: the suspension after above-mentioned ultrasonication is evaporated to AmL, obtain AmL concentrated solution; In 16000r/min, centrifugal 8min under 5 DEG C of conditions, get supernatant liquor, in supernatant liquor, add 95% ethanol be settled to AmL;
The absorption of step 5, total triterpene and purifying: with the flow velocity of 2BV/h, the liquid after above-mentioned fixed appearance being crossed macroporous adsorbent resin column chromatography, with 80% ethanol elution, collects the solution eluted after variable color, the solution eluted is extracting substance.
Table 1 Different Extraction Method is on the impact of the fine pore fungi total triterpene extraction yield of birch
Claims (6)
1. the fine pore fungi total triterpene extracting method of birch, it is characterised in that comprise the steps:
Step 1, pre-treatment: the fine pore fungi mycelia of birch under 60-80 DEG C of condition, dry 10-16 hour;
Step 2, broken wall: pulverized by fine for above-mentioned pretreated birch pore fungi mycelia broken wall, cross 200 order sieves, add 95% ethanol, and the mass ratio of 95% ethanol and mycelia is 30-50:1, is mixed with suspension, soaks 24h;
Step 3, ultrasonication: by fine for above-mentioned birch pore fungi suspension ultrasonication, 60-80 DEG C, power 400W, time 10-20min;
Step 4, concentrating under reduced pressure: the suspension after above-mentioned ultrasonication is evaporated to AmL, obtain AmL concentrated solution; Under 13000-16000r/min, 0-5 DEG C of condition, centrifugal 8-15min, gets supernatant liquor, adds 95% ethanol and be settled to AmL in supernatant liquor;
The absorption of step 5, total triterpene and purifying: with the flow velocity of 2BV/h, the liquid after above-mentioned fixed appearance being crossed macroporous adsorbent resin column chromatography, with 80% ethanol elution, collects the solution eluted after variable color, the solution eluted is extracting substance.
2. the fine pore fungi total triterpene extracting method of a kind of birch according to claim 1, it is characterised in that in described step 1, under 70 DEG C of conditions, dry 12 hours.
3. the fine pore fungi total triterpene extracting method of a kind of birch according to claim 1, it is characterised in that in described step 2,
The mass ratio of 95% ethanol and mycelia is 40:1.
4. the fine pore fungi total triterpene extracting method of a kind of birch according to claim 1, it is characterised in that in described step 3,70 DEG C, power 400W, time 15min.
5. the fine pore fungi total triterpene extracting method of a kind of birch according to claim 1, it is characterised in that in described step 4, in 14000r/min, centrifugal 10min under 0 DEG C of condition.
6. according to the fine pore fungi total triterpene extracting method of a kind of birch according to claim 1, it is characterised in that in described step 5, the post bed diameter of macroporous adsorptive resins is 1.5cm, and post length is 50cm; Macroporous adsorptive resins carries out pre-treatment, with 95% alcohol immersion 24h, more not muddy when the volume ratio being washed till effluent liquid and water with 95% ethanol is 1:5, wash with water afterwards to without alcohol taste, being finally washed to neutrality.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107142219A (en) * | 2017-06-23 | 2017-09-08 | 山东大学 | One plant production triterpene compound drip hole bacterium and its application |
| CN110075132A (en) * | 2019-05-08 | 2019-08-02 | 山西大学 | A kind of method of extraction purification Inonotus obliquus triterpene |
| CN113633668A (en) * | 2021-09-20 | 2021-11-12 | 黑龙江八一农垦大学 | High-efficiency extraction method of total triterpenoids of inonotus obliquus and preparation method of fine powder of total triterpenoids |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101849973A (en) * | 2010-06-11 | 2010-10-06 | 天津大学 | Total triterpenoid extract of inonotus obliquus with hypoglycemic function and pharmaceutical preparation thereof |
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2016
- 2016-03-25 CN CN201610179537.8A patent/CN105663178A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101849973A (en) * | 2010-06-11 | 2010-10-06 | 天津大学 | Total triterpenoid extract of inonotus obliquus with hypoglycemic function and pharmaceutical preparation thereof |
Non-Patent Citations (1)
| Title |
|---|
| 郭辉: "响应面法优化元蘑总三萜提取及大孔树脂纯化工艺研究", 《食品工业》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107142219A (en) * | 2017-06-23 | 2017-09-08 | 山东大学 | One plant production triterpene compound drip hole bacterium and its application |
| CN107142219B (en) * | 2017-06-23 | 2020-06-30 | 山东大学 | Tricholoma trichomonaum for producing triterpenoids and application thereof |
| CN110075132A (en) * | 2019-05-08 | 2019-08-02 | 山西大学 | A kind of method of extraction purification Inonotus obliquus triterpene |
| CN113633668A (en) * | 2021-09-20 | 2021-11-12 | 黑龙江八一农垦大学 | High-efficiency extraction method of total triterpenoids of inonotus obliquus and preparation method of fine powder of total triterpenoids |
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Application publication date: 20160615 |