CN100452990C - Extraction method for primary active matter of edible fungi - Google Patents
Extraction method for primary active matter of edible fungi Download PDFInfo
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- CN100452990C CN100452990C CNB200610123109XA CN200610123109A CN100452990C CN 100452990 C CN100452990 C CN 100452990C CN B200610123109X A CNB200610123109X A CN B200610123109XA CN 200610123109 A CN200610123109 A CN 200610123109A CN 100452990 C CN100452990 C CN 100452990C
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Abstract
A low-temp (lower than 20 deg.C) process for extracting the original-state active components from edible fungus includes such steps as dewatering, breaking, extracting in oil, extracting in alcohol, extracting in water, ultrafiltering, drying, mixing and cold storage.
Description
[technical field]
The invention belongs to the preparation field of edible mushroom extract.
[background technology]
Contain multiple bioactive ingredients in the edible mushroom, the common multiple compositions such as polysaccharide, triterpenes, sterols, glucoside, macrolides, polypeptide class, alkaloid, flavonoids, grease class that comprise.Because function such as these active materials have oxidation-resisting and caducity more, improve immunity, angiocardiopathy preventing and be subjected to popular favor day by day, so the research of active material extracting method also causes people's extensive concern in the edible mushroom.Traditional extracting method mainly contains decocting method and infusion process, decocting method is that material is pulverized the back according to an amount of clear water of the different addings of quality, fully soaked into 1～2 hour, decoct boiling 1～2 hour then, the material slag repeats above step 2～3 time again after the coarse filtration, at last all filtrates is left standstill and smart filter obtains extract; Infusion process is material to be pulverized the back add proper amount of solvent (as: water, ethanol, benzinum etc.) according to quality, and (cold soaking at normal temperatures at normal temperature or constant temperature; Hot dipping is if solvent is that ethanol is at 40～60 ℃, if solvent is that water is at 60～80 ℃) airtight dipping 6～24 hours down, stir in good time, separate then, squeeze, filter extract.Identical with decocting method, extract adopts baking and air-dry method concentrate drying usually.There are many obvious defects in traditional extracting method: 1, active material has water miscible (as: alkaloid salt, flavones etc.), (as: grease, the sterol etc.) that pure dissolubility is arranged, fat-soluble (as: terpene, free alkaloid, glucoside etc.) are arranged, so single extract only extracts the part active material, causes the loss of other active ingredients; 2, chemical reactions such as complexing, hydrolysis, oxidation, reduction take place easily, primitive component is changed when temperature is higher between each composition; When 3, being solvent extraction with water under the normal temperature, enzymolysis takes place and goes bad because of microbial reproduction in extract easily; Volatile when 4, benzinum and ethanol temperature are higher, even the danger that has steam generation to burn.
[summary of the invention]
The present invention aims to provide the extraction method for primary of active matter of edible fungi, and this method can suppress degradations such as the hydrolysis, enzymolysis to the organism component in leaching process; And under the situation that need not add anticorrisive agent, avoided interference and the harm of microbial reproduction to extracting in the leaching process; Can extract simultaneously the active material of edible mushroom fully.
Extracting method of the present invention, its process is as follows:
1, raw material low temperature dewatering
Adopt freezing and method negative pressure, fresh edible fungi raw materials is dehydrated.
2, cooling is pulverized
Adopt the water-cooled pulverizer, be controlled at below 20 ℃ and pulverize edible fungi raw materials.
3, low temperature (＜20 ℃) fat is carried
Preferred benzinum of this step or glycerine or ether are solvent, and the solvent volume consumption is 2～5 times of edible mushroom volumes, and the liposoluble constituent in the edible fungi raw materials is pulverized in lixiviate, add ultrasonic oscillation, accelerate cellular content and separate out.Use the filter paper suction filtration after lixiviate 1-4 hour.Repeat lixiviate filter residue 1-2 time, merging filtrate dries in the shade filter residue slightly.
4, low temperature (＜20 ℃) alcohol extracting
This step preferred alcohol is a solvent, and the solvent volume consumption is 2～5 times of edible fungi raw materials volumes, and the pure soluble components in the edible fungi raw materials is pulverized in lixiviate.Utilize the intermiscibility of ethanol and fat extraction solvent, can wait above-mentioned filter residue to parch.Add ultrasonic oscillation, accelerate cellular content and separate out.Use the filter paper suction filtration after lixiviate 1-4 hour.Repeat lixiviate filter residue 1-2 time, merging filtrate dries in the shade filter residue slightly.
5, low temperature (0～10 ℃) water is carried
The employing pure water is a solvent, and the solvent volume consumption is 2～5 times of edible mushroom volume, and the water soluble ingredient in the edible fungi raw materials is pulverized in lixiviate.Above-mentioned filter residue is added an amount of pure water lixiviate, utilize the intermiscibility of pure extraction solvent and water, can wait filter residue to parch.Add ultrasonic oscillation, accelerate cellular content and separate out.Use the filter paper suction filtration after lixiviate 1-4 hour.Repetitive operation 1-2 time, merging filtrate.
6, ultra-filtration and separation
Employing can tolerate the ultrafiltration apparatus of organic solvent, and molecular weight in the filtrate of extracting less than 6000 with greater than 2,000,000 daltonian compositions removals, is got concentrate.
7, freeze drying
With freeze drier with isolated concentrate drying after, be temporary in drying basin.
8, low-temperature mixed
The product of three kinds of leach extraction methods is being mixed with pulverizer below 20 ℃.
9, freezing
Finished product is loaded on nitrogen-filled seal in glass or the plastic containers, preservation below-15 ℃.
The present invention is on the basis of infusion process, carries out the comprehensive innovation from the structure to the program, from the condition to the target.Adopt the condition of omnidistance low temperature, basic controlling chemical reactions such as hydrolysis, enzymolysis, suppressed the breeding of microorganism and the volatilization of organic solvent, for remedying the defective that dissolution rate under the low temperature reduces, the using ultrasound the resonance method strengthens dissolution rate during dipping simultaneously.According to the intermiscibility between ether and alcohol, alcohol and the water, and ether, alcohol are to the inhibitory or killing effect characteristics of microorganism, employing is mentioned the order that alcohol extracting carries to water again from fat and is carried out continuous extraction operation, not only increased recovery rate, shortened total extraction time, got rid of the interference and the harm of external microbe, also can further keep the prototype structure state of active material in the edible mushroom, to keep its natural pharmacological action.
Extracting method of the present invention mainly contains following advantage:
1, the whole process of active material extraction in the edible mushroom, comprise dehydration, pulverizing, lixiviate, separation, the drying and preservation operation of material, be controlled under the low-temperature condition and carry out.Compare with the traditional extraction process that adopts high temperature or normal temperature condition, suppressed degradations such as hydrolysis, enzymolysis the organism component.Simultaneously, under the situation that need not add anticorrisive agent, avoid interference and the harm of microbial reproduction to extracting in the leaching process, also can reduce the volatilization of organic solvent.
2, document is pointed out, through water carry, after alcohol extracting and fat carries, the most soluble components in the edible mushroom can disengage.So we directly are combined into three extraction methods with these three kinds of extracting methods, carry out continued operation according in twos intermiscibility between solvent, adjust lixiviate order (fat carry → alcohol extracting → water carry), shorten extraction time, reduce the chance of microbial infection leaching liquor.
3, extract is separated by the molecular weight size, remove the main little molecule that plays trophism such as water, inorganic salts, monose, and human body such as the fiber substance big molecule that is difficult to digest and assimilate, improve the purity of active material.
4, extract by low temperature extraction and three, make bioactive extracts go up structure and the assembled state that keeps original largely.The raw material of traditional Chinese medicine theory such as meeting organism balance, polynary cooperation is provided for research, production.
[description of drawings]
Fig. 1 is the expression flow chart that extracts the active material method from edible mushroom of the present invention.
[specific embodiment]
Embodiment 1:
1, the extraction of full active components of glossy ganoderma
In 18 ℃ air-conditioned workshop with full glossy ganoderma (glossy ganoderma processed goods, powdery) (Guangdong Yuewei edible mushroom Technology Co., Ltd.'s production) 1kg adding 3L benzinum flooded 1 hour in the ultrasonic washing groove, filter, filter residue adds and refilters after the 1L benzinum embathes, repetitive operation once, merging filtrate with ultrafiltration apparatus concentrate concentrate, concentrate is temporary in drying basin with the dried product of freeze drier (A).Adding 3L 95% ethanol after filter residue dried in the shade 1 hour flooded 2 hours in the ultrasonic washing groove, filter, filter residue respectively adds at twice and refilters after 1L ethanol embathes, merging filtrate with ultrafiltration apparatus concentrate concentrate, concentrate is temporary in drying basin with the dried product of freeze drier (B).Add 3L after filter residue dried in the shade 1 hour and be cooled to 4 ℃ pure water dipping 2 hours in the ultrasonic washing groove that moves into 4 ℃ of refrigerators through refrigerator, filter, filter residue respectively adds at twice and refilters after 1L low temperature pure water embathes, merging filtrate with ultrafiltration apparatus concentrate concentrate, concentrate with freeze drier dry product (C).With product (A), (B), (C) after the freeze drying of pulverizer mixed concentrated liquid, get the 216g extract, be loaded on nitrogen-filled seal in the vial ,-20 ℃ of refrigerator preservations.
2, contrast experiment
Put forward the method for thick polysaccharide with traditional water and extract the active component of above-mentioned full glossy ganoderma, and itself and the resultant full active components of glossy ganoderma of the invention described above are compared, its result is as follows:
As seen from the above table, extract yield of full glossy ganoderma and function test positive rate are all than the conventional extracting method height of correspondence, and the activated species of constituent analysis obviously increases.
Embodiment 2:
1, rainbow conk extraction of active ingredients
The dry fructification of rainbow conk (mushroom body) is pulverized under 18 ℃ of conditions with the water-cooled Lowtemperaturepulverizer of adorning 40 mesh sieves.In 18 ℃ air-conditioned workshop manyzoned polypore sporophore powder 1kg being added the 1.5L benzinum flooded 1 hour in the ultrasonic washing groove, filter, filter residue adds and refilters after the 1L benzinum embathes, repetitive operation once, merging filtrate with ultrafiltration apparatus concentrate concentrate, concentrate is temporary in drying basin with the dried product of freeze drier (A).Adding 1.5L 95% ethanol after filter residue dried in the shade 1 hour flooded 2 hours in the ultrasonic washing groove, filter, filter residue respectively adds at twice and refilters after 1L ethanol embathes, merging filtrate with ultrafiltration apparatus concentrate concentrate, concentrate is temporary in drying basin with the dried product of freeze drier (B).Add 1.5L after filter residue dried in the shade 1 hour and be cooled to 4 ℃ pure water dipping 2 hours in the ultrasonic washing groove that moves into 4 ℃ of refrigerators through refrigerator, filter, filter residue respectively adds at twice and refilters after 1L low temperature pure water embathes, merging filtrate with ultrafiltration apparatus concentrate concentrate, concentrate gets product (C) after using the freeze drier drying, with the dried product of pulverizer mixed freezing (A), (B), (C), gets the 48g extract, be loaded on nitrogen-filled seal in the vial ,-20 ℃ of refrigerator preservations.
2, contrast experiment
The method of carrying thick polysaccharide with traditional water is extracted the active component of above-mentioned rainbow conk, and itself and the resultant rainbow conk active component of the invention described above are compared, and its result is as follows:
As seen from the above table, all than the conventional extracting method height of correspondence, the activated species of constituent analysis obviously increases for the extract yield of rainbow conk and function test positive rate.
Embodiment 3:
1, mushroom extraction of active ingredients
New fresh mushroom was dewatered in quick freezing unit 6 hours, under 18 ℃ of conditions, mushroom fruiting body (mushroom body) is pulverized with the water-cooled Lowtemperaturepulverizer of adorning 20 mesh sieves.In 18 ℃ air-conditioned workshop mushroom fruiting body powder 1kg being added the 2L benzinum flooded 1 hour in the ultrasonic washing groove, filter, filter residue respectively adds at twice and refilters after the 1L benzinum embathes, merging filtrate with ultrafiltration apparatus concentrate concentrate, concentrate is temporary in drying basin with the dried product of freeze drier (A).Adding 2L 95% ethanol after filter residue dried in the shade 1 hour flooded 2 hours in the ultrasonic washing groove, filter, filter residue respectively adds at twice and refilters after 1L ethanol embathes, merging filtrate with ultrafiltration apparatus concentrate concentrate, concentrate is temporary in drying basin with the dried product of freeze drier (B).Add 2L after filter residue dried in the shade 1 hour and be cooled to 4 ℃ pure water dipping 2 hours in the ultrasonic washing groove that moves into 4 ℃ of refrigerators through refrigerator, filter, filter residue respectively adds at twice and refilters after 1L low temperature pure water embathes, merging filtrate with ultrafiltration apparatus concentrate concentrate, concentrate with freeze drier dry product (C).With the dried product of pulverizer mixed freezing (A), (B), (C), get the 133g extract, be loaded on nitrogen-filled seal in the vial ,-20 ℃ of refrigerator preservations.
2, contrast experiment
The method of carrying thick polysaccharide with traditional water is extracted the active component of above-mentioned mushroom, and itself and the resultant mushroom active component of the invention described above are compared, and its result is as follows:
As seen from the above table, all than the conventional extracting method height of correspondence, the activated species of constituent analysis obviously increases for the extract yield of mushroom and function test positive rate.
Claims (7)
1, the extraction method for primary of active matter of edible fungi, comprise that edible mushroom dehydration pulverizing, extraction, extracting liquid filtering concentrate the also process of preservation, it is characterized in that whole process all carries out in the low temperature below 20 ℃, and carry out successively that alcohol extracting, ester are carried, water is carried, mix after alcohol extract, ester extract, water extract filtering and concentrating and the freeze drying with gained respectively again; Wherein, the solvent that fat is carried is a benzinum, and the solvent of alcohol extracting is an ethanol, and water is carried in 0～10 ℃ and being carried out.
2, extracting method as claimed in claim 1 is characterized in that whole process dewaters to put forward step and all carry out in 18 ℃ outward.
3, extracting method as claimed in claim 1, it is characterized in that water is carried in 4 ℃ carries out.
4, extracting method as claimed in claim 1 is characterized in that fat is carried, alcohol is mentioned the extraction solvent that water is carried volumetric usage respectively is 2～5 times of volume of material.
5, extracting method as claimed in claim 1 is characterized in that fat is carried, alcohol mentions in the leaching process that water carries and all add ultrasonic oscillation.
6, extracting method as claimed in claim 1, the filtration step that it is characterized in that extract adopts ultrafiltration apparatus difference ultrafiltration fat extract, alcohol extract and the water extract that can tolerate organic solvent, and molecular weight is less than 6000 with greater than 2,000,000 daltonian compositions in the removal extract.
7, extracting method as claimed in claim 1 is characterized in that mixed extraction product places below-15 ℃, the inflated with nitrogen preservation.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB200610123109XA CN100452990C (en) | 2006-10-31 | 2006-10-31 | Extraction method for primary active matter of edible fungi |
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| CNB200610123109XA CN100452990C (en) | 2006-10-31 | 2006-10-31 | Extraction method for primary active matter of edible fungi |
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| CN1947732A CN1947732A (en) | 2007-04-18 |
| CN100452990C true CN100452990C (en) | 2009-01-21 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103131195B (en) * | 2013-02-04 | 2015-04-08 | 戴群 | Matsutake active extractives and preparation method and application thereof |
| CN103251035A (en) * | 2013-03-26 | 2013-08-21 | 浦北县健翔食品厂 | Preparation method of Russulasp. powder |
| CN104256564B (en) * | 2014-08-27 | 2016-05-25 | 金湘范 | The former dew of a kind of fungi plant, preparation method and application |
| CN104739890B (en) * | 2015-04-09 | 2018-07-24 | 四川农业大学 | A kind of method of active material in ultrasound assisted extraction edible fungus cluster |
| CN105998090A (en) * | 2016-05-20 | 2016-10-12 | 广东省微生物研究所 | Antitumor active substance extracted from edible fungi of Ganoderma lucidum, and extraction method and application of antitumor active substance |
| CN107373306A (en) * | 2017-07-31 | 2017-11-24 | 广西健美乐食品有限公司 | A kind of preparation method of Russulasp. powder |
| CN108379306A (en) * | 2018-04-25 | 2018-08-10 | 广东省微生物研究所 | A kind of preparation method and the oral solution of Sparassis crispa compound anti-oxidation oral solution |
| CN112159803A (en) * | 2020-10-14 | 2021-01-01 | 潍坊医学院 | Method for extracting beta-glucosidase from lentinus edodes for synthesizing salidroside |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1041106A (en) * | 1988-09-10 | 1990-04-11 | 李绪滨 | A kind of production technology of Ganoderma essence |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1041106A (en) * | 1988-09-10 | 1990-04-11 | 李绪滨 | A kind of production technology of Ganoderma essence |
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Application publication date: 20070418 Assignee: GUANGDONG YUEWEI EDIBLE FUNGI TECHNOLOGY Co.,Ltd. Assignor: Guangdong Institute of Microbiology Contract record no.: 2013440000549 Denomination of invention: Extraction method for primary active matter of edible fungi Granted publication date: 20090121 License type: Exclusive License Record date: 20131223 |
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Address after: 510070 No. 100 martyrs Middle Road, Guangdong, Guangzhou Patentee after: GUANGDONG INSTITUTE OF MICROBIOLOGY (GUANGDONG DETECTION CENTER OF MICROBIOLOGY) Address before: 510070 No. 100 martyrs Middle Road, Guangdong, Guangzhou Patentee before: Guangdong Institute of Microbiology |
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Granted publication date: 20090121 Termination date: 20211031 |