CN105754002B - A kind of preparation method of high content silver fungus polysaccharides - Google Patents
A kind of preparation method of high content silver fungus polysaccharides Download PDFInfo
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- CN105754002B CN105754002B CN201610281501.0A CN201610281501A CN105754002B CN 105754002 B CN105754002 B CN 105754002B CN 201610281501 A CN201610281501 A CN 201610281501A CN 105754002 B CN105754002 B CN 105754002B
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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Abstract
The invention discloses a kind of preparation methods of high content silver fungus polysaccharides, first using the purification step by macroreticular resin twice after heating and refluxing extraction, then in turn through be concentrated under reduced pressure, 95% ethyl alcohol alcohol precipitation, technological process standing, filtering, be dried under reduced pressure, finally crush obtain the extract of tremella polysaccharides, two different macroporous absorbent resin method for combined use effectively eliminate pigment, protein and other impurities in tremella polysaccharides, so as to obtain the tremella polysaccharides of high-content；And it can be used repeatedly for large pore resin absorption column, and resource has not only rationally been utilized but also has saved cost, therefore this method is easy to spread, has very strong practicability, amplifies suitable for production, and raw materials used and by-product is environment-protecting and non-poisonous, is worthy to be popularized.
Description
Technical field
The present invention relates to the extraction preparation fields of plant, are specifically related to a kind of preparation method of high content silver fungus polysaccharides.
Background technology
White fungus is the fructification of Heterobasidiomycetae Tremellaceae white fungus, also known as tremella, tremella etc..Belong to Mycophyta
Tremellaceae Tremella, there is the laudatory title of " hat in bacterium ", and the plantation in China is more universal.Tremella polysaccharides be from Tremella fructification or
A kind of active polysaccharide extracted in spore.Domestic and international numerous studies prove that there is tremella polysaccharides excellent raising human body to exempt from
The physiological actions such as epidemic disease function, antiviral, antitumor, antiulcer, reducing blood lipid, hypoglycemic, norcholesterol, and tremella polysaccharides have
Extremely strong performance of keeping humidity and thickening stabilities is applied as natural moisture preserving agent and is widely paid attention in daily chemicals field.Therefore
Rationally it is of great significance using the extraction and purification process of white fungus resource and research tremella polysaccharides.
A kind of white fungus intracellular polyse separation of Chinese patent (application No. is 201410796766.5), the method for purifying, pass through
Enzymolysis, ultrasonic extraction, concentration, alcohol precipitation obtain the crude extract of tremella polysaccharides；The crude extract of tremella polysaccharides using ultrasonic dissolution,
D101 resins column chromatography, DEAE celluosic resins are detached, are concentrated, are dried to obtain tremella polysaccharides.This method is carried due to enzyme process
Tremella polysaccharides is taken to require reaction process stringent, operating technology is more demanding, and the more multipair equipment of the method processing step will
It asks high, causes production cost high, therefore be not suitable with mass production.
The preparation method of Chinese patent (application No. is 201510336334.0) tremella polysaccharides, the invention pass through Ultramicro-powder
Broken, ultrasonic extraction, Sevage reagents deproteinized, peroxide passivation decoloration, obtains tremella polysaccharides at alcohol precipitation.The method use a large amount of
Various organic solvents, not only production cost is high and chloroform toxicity is larger, is also not suitable with mass production.
A kind of simple for process, the research result that environmental protection low cost is suitable for the preparation method of the tremella polysaccharides of mass production must be visited
It begs for.
Invention content
Goal of the invention：The preparation method of tremella polysaccharides in the prior art is of high cost, complex process in order to overcome, and makes
The problem of not being suitable for large batch of industrial production not environmentally with raw material, the present invention propose a kind of simple for process, environmental protection, cost
It is low, it is applicable to production amplification, the preparation method of the high content silver fungus polysaccharides easy to spread with very strong practicability.
Technical solution：In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：A kind of high-content white fungus
The preparation method of polysaccharide, includes the following steps：
(1) white fungus to be extracted is taken to be put into extraction kettle, the extraction that water is heated to reflux carrying out 2-4 times is added in, heats every time
The time of refluxing extraction is 1-3h, and extracting solution filtering merges multiple extracting solution, spare；The wherein quality of white fungus and the volume of water
Than being 1:50-1:200；
(2) take No. 1 macroporous resin column on the mixture of extracting solution that step (1) obtains, after the completion of upper prop, with purified water into
Row is eluted to efflux and can't detect polysaccharide, stops elution, collects eluent, spare；Wherein the volume of elution purified water is used
Measure 2-6 times for white fungus quality in step (1)；
(3) it takes No. 2 macroporous resin columns on the eluent that step (2) obtains, after the completion of upper prop, is eluted to purified water
Efflux can't detect polysaccharide, stop elution, collect eluent, spare；The volumetric usage of wherein elution purified water is step
(1) 2-6 times of white fungus quality in；
(4) eluent of step (3) is taken to add in white fungus quality 6-18 volumes in step (1) after being concentrated under reduced pressure at 60-78 DEG C
95% ethyl alcohol, concentration volume is 2-6 times of white fungus quality in step (1)；Stand 6-24h, filtering, at 60-78 DEG C
At a temperature of be dried under reduced pressure, required tremella polysaccharides are obtained after crushing.
More preferably, extraction time is 3 times in the step (1), and time of each heating and refluxing extraction is 2h, white fungus
Quality and water volume ratio be 1:100.
More preferably, No. 1 macroreticular resin model HPD-500, HPD-600, LX-11, LX-60 in the step (2)
In one kind.
Further, No. 1 macroreticular resin model LX-60.
More preferably, one kind in the step (3) in No. 2 macroreticular resin models HPD-100, LX-10, LX-8.
Further, No. 2 macroreticular resin models LX-10.
More preferably, in the step (2), (3) volumetric usage of elution purified water be white fungus in step (1) matter
4 times of amount.
More preferably, the detection of polysaccharide uses alphanaphthol reaction in the step (2), (3).
More preferably, the temperature for being concentrated under reduced pressure and being dried under reduced pressure in the step (4) is 70 DEG C, the body of 95% ethyl alcohol
Product dosage is 12 times of the quality of white fungus in step (1).
More preferably, the mesh number crushed in the step (4) is 60-100 mesh.
Advantageous effect：A kind of preparation method of high content silver fungus polysaccharides provided by the invention uses be heated to reflux carrying first
By the purification step of macroreticular resin twice after taking, then in turn through be concentrated under reduced pressure, 95% ethyl alcohol alcohol precipitation, standing, filtering,
The technological process be dried under reduced pressure, finally crushed obtains the extract of tremella polysaccharides, two different macroporous absorbent resin combination sides
Method effectively eliminates pigment, protein and other impurities in tremella polysaccharides, so as to obtain the tremella polysaccharides of high-content；It is and big
It can be used repeatedly for macroporous adsorbent resin column, and resource has not only rationally been utilized but also has saved cost, therefore this method is easy to spread, has had
Very strong practicability amplifies, and raw materials used and by-product is environment-protecting and non-poisonous, is worthy to be popularized suitable for production.
Specific embodiment
With reference to embodiment, the present invention is described in further detail：
Reagent and drug：
White fungus used is purchased from Hubei, assay control dextrose standard sample, purchased from Aladdin, institute in following embodiment
Ethyl alcohol with 95% is that analysis is pure, and water is purified water, other solvents are pure to analyze, and auxiliary material used is pharmaceutical grade.
Embodiment 1：
A kind of preparation method of high content silver fungus polysaccharides, includes the following steps：
(1) commercially available white fungus 1kg is taken to be put into extraction kettle, adds in the purified water of 100L, is heated to reflux carrying out the extraction of 2 times,
The time of each heating and refluxing extraction is 2h, is uniformly mixed and merges after extracting solution filtering twice, spare；
(2) it takes No. 1 macroporous resin column LX-60 on the mixture of extracting solution that step (1) obtains, after the completion of upper prop, uses 4L
Purified water be eluted to efflux and can't detect polysaccharide, stop elution, collect eluent, it is spare；The wherein detection of polysaccharide
Using alphanaphthol reaction；
(3) No. 2 macroporous resin column LX-10 on the eluent that step (2) obtains are taken, after the completion of upper prop, with the purified water of 4L
Be eluted to efflux and can't detect polysaccharide, stop elution, collect eluent, it is spare；Wherein the detection of polysaccharide uses α-naphthalene
Phenol reacts；
(4) eluent of step (3) is taken to be concentrated under reduced pressure into 4L at 70 DEG C, slowly stirring adds in 95% ethyl alcohol of 12L,
12h is stood, filtering is dried under reduced pressure at the temperature at 70 DEG C, is crushed to after 80 mesh that obtain the white fungus that UV contents are 97.8% more
Sugared 203.5g, wherein measurement of the polysaccharide content use sulfuric acid-phynol method.
Wherein, step (2) and the sequence of (3) can overturn progress.
Embodiment 2：
A kind of preparation method of high content silver fungus polysaccharides, includes the following steps：
(1) commercially available white fungus 1kg is taken to be put into extraction kettle, adds in the purified water of 100L, is heated to reflux carrying out the extraction of 2 times,
The time of each heating and refluxing extraction is 2h, is uniformly mixed and merges after extracting solution filtering twice, spare；
(2) it takes No. 1 macroporous resin column LX-60 on the mixture of extracting solution that step (1) obtains, after the completion of upper prop, uses 4L
Purified water be eluted to efflux and can't detect polysaccharide, stop elution, collect eluent, it is spare；The wherein detection of polysaccharide
Using alphanaphthol reaction；
(3) No. 2 macroporous resin column LX-10 on the eluent that step (2) obtains are taken, after the completion of upper prop, with the purified water of 4L
Be eluted to efflux and can't detect polysaccharide, stop elution, collect eluent, it is spare；Wherein the detection of polysaccharide uses α-naphthalene
Phenol reacts；
(4) eluent of step (3) is taken to be concentrated under reduced pressure into 8L at 70 DEG C, slowly stirring adds in 95% ethyl alcohol of 24L,
It stands for 24 hours, filtering is dried under reduced pressure at the temperature at 70 DEG C, is crushed to after 60 mesh that obtain the white fungus that UV contents are 92.1% more
Sugared 387.5g；Wherein measurement of the polysaccharide content uses sulfuric acid-phynol method.
Wherein, step (2) and the sequence of (3) can overturn progress.
Embodiment 3：
A kind of preparation method of high content silver fungus polysaccharides, includes the following steps：
(1) commercially available white fungus 0.5kg is taken to be put into extraction kettle, adds in the purified water of 100L, is heated to reflux carrying out 4 times and carries
It takes, the time of each heating and refluxing extraction is 3h, is uniformly mixed and merges after extracting solution filtering twice, spare；
(2) it takes No. 1 macroporous resin column HPD-500 on the mixture of extracting solution that step (1) obtains, after the completion of upper prop, uses
The purified water of 3L be eluted to efflux and can't detect polysaccharide, stops elution, collects eluent, spare；The wherein inspection of polysaccharide
It surveys using alphanaphthol reaction；
(3) No. 2 macroporous resin column HPD-100 on the eluent that step (2) obtains are taken, after the completion of upper prop, with the purifying of 3L
Water be eluted to efflux and can't detect polysaccharide, stops elution, collects eluent, spare；Wherein the detection of polysaccharide using α-
Naphthol reaction；
(4) eluent of step (3) is taken to be concentrated under reduced pressure into 3L at 70 DEG C, slowly stirring adds in 95% ethyl alcohol of 60L,
6h is stood, filtering is dried under reduced pressure at the temperature at 70 DEG C, is crushed to after 100 mesh that obtain the white fungus that UV contents are 91.1% more
Sugared 214.6g；Wherein measurement of the polysaccharide content uses sulfuric acid-phynol method.
Wherein, step (2) and the sequence of (3) can overturn progress.
It can be seen that a kind of preparation method of high content silver fungus polysaccharides provided by the invention from the data of embodiment 1-3, lead to
Cross that two different macroporous absorbent resin method for combined use effectively eliminate pigment in tremella polysaccharides, protein and other are miscellaneous
Matter, so as to obtain the tremella polysaccharides of high-content；And it can be used repeatedly for large pore resin absorption column, and resource has not only rationally been utilized but also has saved
About cost, therefore this method is easy to spread, has very strong practicability, amplifies suitable for production, and raw materials used and secondary
Product is environment-protecting and non-poisonous, is worthy to be popularized.
It should be pointed out that more than specific embodiment is only illustrative of the invention and is not intended to limit the scope of the invention,
After having read the present invention, those skilled in the art fall within the modification of the various equivalent forms of the present invention power appended by the application
Profit requires limited range.
Claims (8)
1. a kind of preparation method of high content silver fungus polysaccharides, it is characterised in that include the following steps：
（1）White fungus to be extracted is taken to be put into extraction kettle, the extraction that water is heated to reflux carrying out 2-4 times is added in, is heated to reflux every time
The time of extraction is 1-3h, and extracting solution filtering merges multiple extracting solution, spare；The wherein quality of white fungus and the volume ratio of water be
1:50-1:200；
（2）Take step（1）No. 1 macroporous resin column on the mixture of obtained extracting solution after the completion of upper prop, is washed with purified water
It takes off to efflux and can't detect polysaccharide, stop elution, collect eluent, it is spare；The volumetric usage of wherein elution purified water is
Step（1）2-6 times of middle white fungus quality；In described No. 1 macroreticular resin model HPD-500, HPD-600, LX-11, LX-60
It is a kind of；
（3）Take step（2）No. 2 macroporous resin columns on obtained eluent after the completion of upper prop, are carried out being eluted to outflow with purified water
Liquid can't detect polysaccharide, stop elution, collect eluent, spare；The volumetric usage of wherein elution purified water is step（1）In
2-6 times of white fungus quality；One kind in described No. 2 macroreticular resin models HPD-100, LX-10, LX-8.
（4）Take step（3）Eluent 60-78 DEG C be concentrated under reduced pressure after add in step（1）The 95% of middle white fungus quality 6-18 volumes
Ethyl alcohol, concentration volume is step（1）2-6 times of middle white fungus quality；6-24h is stood, is filtered, at the temperature at 60-78 DEG C
It is dried under reduced pressure, required tremella polysaccharides is obtained after crushing.
2. the preparation method of high content silver fungus polysaccharides according to claim 1, it is characterised in that：The step（1）In carry
It is 3 times to take number, and the time of each heating and refluxing extraction is 2h, and the quality of white fungus and the volume ratio of water are 1:100.
3. the preparation method of high content silver fungus polysaccharides according to claim 1, it is characterised in that：No. 1 macroreticular resin
Model LX-60.
4. the preparation method of high content silver fungus polysaccharides according to claim 1, it is characterised in that：No. 2 macroreticular resins
Model LX-10.
5. the preparation method of high content silver fungus polysaccharides according to claim 1, it is characterised in that：The step（2）、（3）
The volumetric usage of middle elution purified water is step（1）4 times of middle white fungus quality.
6. the preparation method of high content silver fungus polysaccharides according to claim 1, it is characterised in that：The step（2）、（3）
The detection of middle polysaccharide uses α-naphthol reaction.
7. the preparation method of high content silver fungus polysaccharides according to claim 1, it is characterised in that：The step（4）In subtract
Pressure concentration and the temperature being dried under reduced pressure are 70 DEG C, and the volumetric usage of 95% ethyl alcohol is step（1）12 times of middle white fungus quality.
8. the preparation method of high content silver fungus polysaccharides according to claim 1, it is characterised in that：The step（4）Middle powder
Broken mesh number is 60-100 mesh.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101434662A (en) * | 2008-12-29 | 2009-05-20 | 河南工业大学 | Method for preparing fungal polysaccharide |
| CN101602652A (en) * | 2009-07-09 | 2009-12-16 | 浙江大学 | A kind of method of from moraceae plants, extracting trans-resveratrol |
| CN105367681A (en) * | 2015-12-16 | 2016-03-02 | 黑龙江众生生物工程有限公司 | Edible and medicinal fungal polysaccharide low-temperature normal-pressure plasma extraction method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101434662A (en) * | 2008-12-29 | 2009-05-20 | 河南工业大学 | Method for preparing fungal polysaccharide |
| CN101602652A (en) * | 2009-07-09 | 2009-12-16 | 浙江大学 | A kind of method of from moraceae plants, extracting trans-resveratrol |
| CN105367681A (en) * | 2015-12-16 | 2016-03-02 | 黑龙江众生生物工程有限公司 | Edible and medicinal fungal polysaccharide low-temperature normal-pressure plasma extraction method |
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