CN110256524A - The extracting method of selenka - Google Patents
The extracting method of selenka Download PDFInfo
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- CN110256524A CN110256524A CN201910653335.6A CN201910653335A CN110256524A CN 110256524 A CN110256524 A CN 110256524A CN 201910653335 A CN201910653335 A CN 201910653335A CN 110256524 A CN110256524 A CN 110256524A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J71/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton is condensed with a heterocyclic ring
- C07J71/0005—Oxygen-containing hetero ring
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention discloses the extracting methods of selenka, include the following steps: (1) supercritical extract: using sea cucumber by-product as raw material, use supercritical carbon dioxide as extractant, beeswax carries out extracting to obtain CO 2 fluid extract liquor as entrainer；By in CO 2 fluid extract liquor carbon dioxide and extract separate, the absorption of extract ethyl alcohol is absorbed liquid；(2) resin adsorption refines: absorbing liquid made from step (1) being carried out adsorption refining using macroporous absorbent resin, uses ethyl alcohol as the effective component of eluent parsing selenka, collection obtains selenka eluent；(3) it decolourizes: the selenka eluent that step (2) obtains being decolourized, is filtered, washed after decoloration, obtains filtered fluid and cleaning solution；(4) it is concentrated and dried to obtain selenka.The present invention is combined supercritical extract with resin adsorption purification, realizes the extraction to selenka, and the purity is high and recovery rate of selenka are high.
Description
Technical field
The present invention relates to Holothurian machining technical fields, and in particular to the extracting method of selenka.
Background technique
Sea cucumber is the general name of Echinodermata Holothuroidea animal, and sea cucumber has nutritive value abundant, wherein selenka
It is the main secondary metabolite and its material base for carrying out chemical defence of sea cucumber.Some researches show that selenka has
Anti-tumor activity, lipid-metabolism adjust activity, glycometabolism adjusts activity, hemolytic activity, antibacterial activity, immune-enhancing activity, guarantor
Protect hemopoietic system functional activity, reduce blood uric acid etc..
Selenka polarity is larger, in soluble easily in water, dilute alcohol, hot methanol and ethyl alcohol, is insoluble in propyl alcohol, is practically insoluble in second
The lipophylic organic solvents such as ether, benzene.Selenka has biggish solubility in aqueous butanol or valeric acid.Therefore, amylalcohol or fourth
Alcohol is frequently as the extractant for separating selenka from aqueous solution, to separate with big ingredients of hydrophilies such as sugar, protein.
Common extracting method has alcohol extracting method and resin adsorption method.General alcohol extracting, which is followed the example of, can be related to ether or petroleum ether
Degreasing, the deproteinized of chloroform, and the step of being saturated with water extracting n-butyl alcohol, being related to be complicated is cumbersome and used
Chemical reagent is more, causes biggish pollution to environment.Macroreticular resin absorbing method generally relates to water and dehydrated alcohol, as
The method of coarse extraction has the disadvantages of operating time is long, organic solvent usage amount is big, at high cost, easy to pollute, is not suitable for industrialization
Production, but the purification step as the later period, the organic solvent being related to is relatively fewer, is relatively suitble to the further of selenka
Purification.
Supercritical extract is that in the supercritical state, supercritical fluid is in contact with the substance to be separated, it is made to have selection
Property polarity size, boiling point height are extracted in turn with the ingredient of molecular size range.It, will be overcritical at present in the field of Chinese medicines
Extraction and resin adsorption method combine the effective component extracted in drug, have preferable extraction effect.
Solid by-product after extracting sea cucumber polypeptide by sea cucumber intestine, does not recycle generally as waste, causes environment
The waste of pollution and resource, selenka can be extracted from the solid by-product after sea cucumber intestine extraction sea cucumber polypeptide, at present also
The correlative study that selenka is not extracted from the solid by-product after sea cucumber intestine extraction sea cucumber polypeptide, will be not overcritical yet
Extraction combines the extraction applied to selenka with resin adsorption method.
Summary of the invention
For the above-mentioned prior art, the object of the present invention is to provide a kind of to extract the solid after sea cucumber polypeptide using sea cucumber intestine
The method of by-product extraction selenka.The present invention is by rationally controlling the combination of supercritical extract and resin adsorption purification
Technological parameter in supercritical extract and resin adsorption subtractive process promotes the two mutually collaboration, realizes to sea cucumber intestine extraction
The extraction of selenka in solid by-product after sea cucumber polypeptide, and keep the purity is high of selenka and recovery rate high；The present invention
Residue of the raw material sources after producing sea cucumber polypeptide, on the one hand realizes the multiple utilization of substance；Still further aspect, raw material
After middle polypeptide removes, it is more advantageous to the extraction of selenka, and eliminate and remove removing protein using organic reagent such as chloroform etc.
Process, raw material have passed through the processing of microorganism when extracting polypeptide, and the substances such as polysaccharide have all been removed substantially, have been further increased
The purity and recovery rate of sea cucumber polypeptide.
To achieve the above object, the present invention adopts the following technical scheme:
The first aspect of the present invention provides a kind of extracting method of selenka, includes the following steps:
(1) supercritical extract: using sea cucumber by-product as raw material, use supercritical carbon dioxide as extractant, beeswax
It carries out extracting to obtain CO 2 fluid extract liquor as entrainer, wherein extraction temperature is 30-45 DEG C, Fluid pressure 20-
40Mpa, flow velocity 0.10-0.40ml/min, extraction time 1-3h；
By the carbon dioxide and the isolated extract of extract progress in CO 2 fluid extract liquor, extract second
Alcohol absorbs the liquid that is absorbed；
(2) resin adsorption refines: absorbing liquid made from step (1) being carried out adsorption refining using macroporous absorbent resin, is used
The ethyl alcohol that mass fraction is 65-75% parses the effective component of selenka as eluent, and collection obtains selenka elution
Liquid；
(3) it decolourizes: decolourizing decolorising agent is added in selenka eluent that step (2) obtains, filtering after decoloration,
Washing, obtains filtered fluid and cleaning solution；
(4) filtered fluid of step (3) and cleaning solution are concentrated and dried to obtain selenka.
Preferably, the ethyl alcohol is 2-3 times, volumetric concentration 20%-40% of CO 2 fluid extract liquor volume, is used
The effect that ethyl alcohol absorbs is except degreasing.
Preferably, the sea cucumber by-product is that sea cucumber intestine extracts the solid by-product after sea cucumber polypeptide, and sea cucumber intestine is derived from not
New fresh sea cucumber by any drying process or the dried sea-cucumber being soaked.In the present invention sea cucumber by-product use application No. is
201811365215.8, sea cucumber intestine disclosed in a kind of entitled production method of sea cucumber polypeptide extracts the solid pair after sea cucumber polypeptide
Product.
Preferably, when step (1), when carbon dioxide and extract separate, separating pressure 7.8-12Mpa, temperature is
32.8-55℃。
Preferably, in step (2), the weight of absorbing liquid applied sample amount is identical as weight resin, absorbing liquid loading flow control
In 2 times per hour of bed volume.
Preferably, in step (2), ethanol elution flow control is in 1-1.2 bed volume per hour.
Preferably, it in step (2), collects and obtains the amount of selenka eluent and be 6-7 times of weight resin and measure.
Preferably, decolorising agent is magnesia in step (3), and the amount of magnesia is added in every 100ml selenka eluent
For 1-5g；Magnesia rear decoloring 1-1.5h is added.
Preferably, step (4) is specifically that the filtered fluid for obtaining step (3) and cleaning solution carry out vacuum-concentrcted, so
After be spray-dried up to selenka.
Preferably, in step (4), thickening temperature≤80 DEG C are concentrated vacuum degree≤- 0.08Mpa, it is relatively close to be concentrated into stiff paste
Degree is 1.1-1.15.
The second aspect of the present invention provides the selenka extracted by said extracted method.
Beneficial effects of the present invention:
(1) present invention is by rationally controlling supercritical extract and tree for the combination of supercritical extract and resin adsorption purification
Technological parameter during rouge adsorption refining promotes the two mutually collaboration, realizes to consolidating after sea cucumber intestine extraction sea cucumber polypeptide
The extraction of selenka in shape by-product, and keep the purity is high of selenka and recovery rate high；Utilize supercritical CO2Extraction, benefit
Use CO2A kind of specialized fluids state under high pressure, selenka as much as possible is extracted from other compositions, still
The ingredient extracted is complex, and especially grease type impurity is more, for this purpose, and then using low-concentration ethanol extracting sea cucumber soap
The ingredients such as glycosides；In order to further refine, by the directly upper macroreticular resin of extract liquor, in order to obtain the higher sea cucumber soap of purity
Glycosides.
(2) supercritical carbon dioxide extracting method, have the advantages that it is nontoxic, avoid environmental pollution, recovery rate high, with resin
After adsorption refining combines, the selenka made is with high purity, recovery rate is high.
(3) during the entire process of the present invention extracts selenka, it is not related to poisonous and harmful organic reagent, ethyl alcohol one is used only
Kind organic reagent, environmentally protective, recovery rate is high, easy to operate, avoids environmental pollution, is suitble to industrialized production.
(4) so that Holothurian machining by-product is turned waste into wealth through the invention, can be effectively reduced pollution, realize to sea cucumber by-product
The recycling and reusing of selenka in object, economizes on resources, and technical solution of the present invention can generate huge economic benefit and society
Meeting benefit, therefore value and wide industrial applications prospect with good practical application.
(5) on the one hand residue of the raw material sources of the present invention after producing sea cucumber polypeptide realizes the multiple benefit of substance
With；Still further aspect is more advantageous to the extraction of selenka, and eliminate and utilize organic reagent after polypeptide removes in raw material
Such as chloroform goes the process of removing protein；Raw material has already passed through the processing of microorganism when extracting polypeptide, and the substances such as polysaccharide are basic
It has all removed, has improved the purity and recovery rate of sea cucumber polypeptide.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
Reagent that the present invention uses, method and apparatus is the art conventional reagents, method and apparatus, except non-specifically saying
Bright, following embodiment agents useful for same and material are commercially available.
Embodiment 1: the extraction of selenka
The following steps are included: (1) supercritical extract: 0.885 kilogram of sea cucumber by-product being imported in 10L extraction kettle, is opened
With supercritical device, supercritical carbon dioxide fluid squeezes into extractor by compressor after being filtered with the flow of 15L/h,
To the pressure 35Mpa for reaching setting, extraction temperature by extractor collet circulation water management and stablize at 35 DEG C, while importing bee
Wax is 35 DEG C, Fluid pressure 35Mpa in extraction temperature as entrainer, and flow velocity is under 0.3ml/min, and extraction 3h is extracted
Object is taken, supercritical carbon dioxide extraction liquid reaches knockout drum decompression, and separating and extracting object pressure is 8Mpa, and temperature is 50 DEG C,
The ethyl alcohol that extract volumetric concentration is 30% absorbs the liquid that is absorbed, wherein for the 2-3 of CO 2 fluid extract liquor volume
Times；CO2Gas enters compressor cycle use；
(2) resin adsorption refine: in absorbing liquid to equipped with macroporous absorbent resin column bed on adsorbed, absorbing liquid loading
Measure, absorbing liquid loading flow control bed volume at per hour 2 times identical as weight resin；With the ethyl alcohol of mass fraction 75%
The effective component of the selenka of resin adsorption is eluted, the amount of selenka eluent is 6-7 times of weight resin, elution flow rate
Control obtains selenka eluent in 1 bed volume per hour, collection；
(3) it decolourizes: the selenka eluent that step (2) obtains is put into bleacher, magnesia is added, wherein often
The amount that magnesia is added in 100ml selenka eluent is 1-5g, is stirred reflux decoloration 1.5h, then carries out sheet frame mistake
Filter, washing, obtain filtered fluid and cleaning solution；
(4) be concentrated and dried: the filtered fluid and cleaning solution that step (3) is obtained carry out vacuum-concentrcted, then do by spraying
It is dry that vacuum degree≤- 0.08Mpa is concentrated in thickening temperature≤80 DEG C up to selenka, be concentrated into stiff paste relative density be 1.1 (
50 DEG C of surveys).Obtained selenka purity is 70%, the rate of recovery 69%.
Embodiment 2: the extraction of selenka
The following steps are included: (1) supercritical extract: 0.89 kilogram of sea cucumber by-product being imported in 10L extraction kettle, is enabled
Supercritical device, supercritical carbon dioxide fluid squeeze into extractor by compressor after being filtered with the flow of 15L/h, until
Reach the pressure 25Mpa of setting, extraction temperature by extractor collet circulation water management and stablize at 40 DEG C, while importing beeswax
It is 40 DEG C, Fluid pressure 25Mpa in extraction temperature as entrainer, flow velocity is under 0.4ml/min, and extraction 2h is extracted
Object, supercritical carbon dioxide extraction liquid reach knockout drum decompression, and separating and extracting object pressure is 10Mpa, and temperature is 40 DEG C, extraction
The ethyl alcohol that object volumetric concentration is 20% is taken to absorb the liquid that is absorbed, wherein ethanol consumption is CO 2 fluid extract liquor volume
2-3 times；CO2Gas enters compressor cycle use；
(2) resin adsorption refine: in absorbing liquid to equipped with macroporous absorbent resin column bed on adsorbed, absorbing liquid loading
Measure, absorbing liquid loading flow control bed volume at per hour 2 times identical as weight resin；With the ethyl alcohol of mass fraction 65%
The selenka effective component of resin adsorption is eluted, the amount of selenka eluent is 6 times of amounts of resin weight, elution flow rate control
In 1.2 bed volumes per hour, collection obtains selenka eluent；
(3) it decolourizes: the selenka eluent that step (2) obtains is put into bleacher, magnesia is added, wherein often
The amount that magnesia is added in 100ml selenka eluent is 1-5g, is stirred reflux decoloration 1.5h, then carries out sheet frame mistake
Filter, washing, obtain filtered fluid and cleaning solution；
(4) be concentrated and dried: the filtered fluid and cleaning solution that step (3) is obtained carry out vacuum-concentrcted, then do by spraying
It is dry that vacuum degree≤- 0.08Mpa is concentrated in thickening temperature≤80 DEG C up to selenka, be concentrated into stiff paste relative density be 1.1 (
50 DEG C of surveys).Obtained selenka purity is 75%, the rate of recovery 71%.
Embodiment 3: the extraction of selenka
The following steps are included: (1) supercritical extract: 0.86 kilogram of sea cucumber by-product being imported in 10L extraction kettle, is enabled
Supercritical device, supercritical carbon dioxide fluid squeeze into extractor by compressor after being filtered with the flow of 15L/h, until
Reach the pressure 20Mpa of setting, extraction temperature by extractor collet circulation water management and stablize at 40 DEG C, while importing beeswax
It is 40 DEG C, Fluid pressure 20Mpa in extraction temperature as entrainer, flow velocity is under 0.2ml/min, and extraction 3h is extracted
Object, supercritical carbon dioxide extraction liquid reach knockout drum decompression, and separating and extracting object pressure is 12Mpa, and temperature is 35 DEG C, extraction
The ethyl alcohol that object volumetric concentration is 40% is taken to absorb the liquid that is absorbed, wherein ethanol consumption is CO 2 fluid extract liquor volume
2-3 times；CO2Gas enters compressor cycle use；
(2) resin adsorption refine: in absorbing liquid to equipped with macroporous absorbent resin column bed on adsorbed, absorbing liquid loading
Measure, absorbing liquid loading flow control bed volume at per hour 2 times identical as weight resin；With mass fraction 65-70%'s
The selenka effective component of ethanol elution resin adsorption, the amount of selenka eluent are that 6-7 times of resin weight is measured, elution stream
Speed control obtains selenka eluent in 1.1 bed volumes per hour, collection；
(3) it decolourizes: the selenka eluent that step (2) obtains is put into bleacher, magnesia is added, wherein often
The amount that magnesia is added in 100ml selenka eluent is 1-5g, is stirred reflux decoloration 1-1.5h, then carries out sheet frame
It is filtered, washed, obtains filtered fluid and cleaning solution；
(4) be concentrated and dried: the filtered fluid and cleaning solution that step (3) is obtained carry out vacuum-concentrcted, then do by spraying
Vacuum degree≤- 0.08Mpa is concentrated in dry selenka to obtain the final product, thickening temperature≤80 DEG C, and being concentrated into stiff paste specific gravity relative density is
(1.1 being surveyed at 50 DEG C).Obtained selenka purity is 79%, the rate of recovery 75%.
From the foregoing, it will be observed that extracting the purity and rate of recovery highest of selenka by embodiment 3.
Comparative example 1: the extraction of selenka
The following steps are included: (1) prepares absorbing liquid: it is 40% that volumetric concentration will be added in 0.86 kilogram of sea cucumber by-product
Ethyl alcohol, filter to obtain absorbing liquid.
(2) resin adsorption refine: in absorbing liquid to equipped with macroporous absorbent resin column bed on adsorbed, absorbing liquid loading
Measure, absorbing liquid loading flow control bed volume at per hour 2 times identical as weight resin；With mass fraction 65-70%'s
The selenka effective component of ethanol elution resin adsorption, the amount of selenka eluent are that 6-7 times of resin weight is measured, elution stream
Speed control obtains selenka eluent in 1.1 bed volumes per hour, collection；
(3) it decolourizes: the selenka eluent that step (2) obtains is put into bleacher, magnesia is added, wherein often
The amount that magnesia is added in 100ml selenka eluent is 1-5g, is stirred reflux decoloration 1-1.5h, then carries out sheet frame
It is filtered, washed, obtains filtered fluid and cleaning solution；
(4) be concentrated and dried: the filtered fluid and cleaning solution that step (3) is obtained carry out vacuum-concentrcted, then do by spraying
Dry selenka to obtain the final product, thickening temperature≤80 DEG C are concentrated vacuum degree≤- 0.08Mpa, are concentrated into stiff paste specific gravity 1.1 (at 50 DEG C
It surveys).Obtained selenka purity is 65%, rate of recovery 20-30%.
Comparative example 1 and the difference of embodiment 3 are do not have supercritical extract process.The sea cucumber extracted by comparative example 1
Saponin(e, purity and the rate of recovery are below each embodiment, therefore the combination of supercritical extract and resin adsorption purification can be bright
The aobvious purity and the rate of recovery for improving selenka.
The foregoing is merely preferred embodiment of the present application, are not intended to limit this application, for the skill of this field
For art personnel, various changes and changes are possible in this application.Within the spirit and principles of this application, made any to repair
Change, equivalent replacement, improvement etc., should be included within the scope of protection of this application.
Claims (10)
1. a kind of extracting method of selenka, which comprises the steps of: (1) supercritical extract: by sea cucumber by-product
Object uses supercritical carbon dioxide as extractant as raw material, and beeswax carries out extracting to obtain CO 2 fluid as entrainer
Extract liquor, wherein extraction temperature is 30-45 DEG C, Fluid pressure 20-40Mpa, flow velocity 0.10-0.40ml/min, when extraction
Between 1-3h；
By in CO 2 fluid extract liquor carbon dioxide and extract carry out isolated extract, extract is inhaled with ethyl alcohol
Receipts are absorbed liquid；
(2) resin adsorption refines: absorbing liquid made from step (1) being carried out adsorption refining using macroporous absorbent resin, uses quality
The ethyl alcohol that score is 65-75% parses the effective component of selenka as eluent, and collection obtains selenka eluent；
(3) it decolourizes: decolourizing decolorising agent is added in selenka eluent that step (2) obtains, filter, wash after decoloration
It washs, obtains filtered fluid and cleaning solution；
(4) filtered fluid of step (3) and cleaning solution are concentrated and dried to obtain selenka.
2. extracting method according to claim 1, it is characterised in that: in step (1), the ethyl alcohol is CO 2 fluid
2-3 times of extract liquor volume, volumetric concentration 20%-40%.
3. extracting method according to claim 1, which is characterized in that in step (1), carbon dioxide and extract separation
When, separating pressure 7.8-12Mpa, temperature is 32.8-55 DEG C.
4. extracting method according to claim 1, which is characterized in that in step (2), the weight of absorbing liquid applied sample amount and tree
Rouge weight is identical, bed volume of the absorbing liquid loading flow control at 2 times per hour.
5. extracting method according to claim 1, which is characterized in that in step (2), ethanol elution flow control is every small
When 1-1.2 bed volume.
6. extracting method according to claim 1, which is characterized in that in step (2), collection obtains selenka eluent
Amount be 6-7 times of weight resin and measure.
7. extracting method according to claim 1, which is characterized in that decolorising agent is magnesia, every 100ml in step (3)
The amount that magnesia is added in selenka eluent is 1-5g；Magnesia rear decoloring 1-1.5h is added.
8. extracting method according to claim 1, which is characterized in that step (4) is specifically the filtering for obtaining step (3)
Liquid and cleaning solution carry out vacuum-concentrcted, are then spray-dried up to selenka.
9. extracting method according to claim 8, which is characterized in that in step (4), thickening temperature≤80 DEG C, concentration is very
Reciprocal of duty cycle≤- 0.08Mpa, being concentrated into stiff paste relative density is 1.1-1.15.
10. the selenka that the described in any item extracting methods of claim 1-9 are extracted.
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| CN110934889A (en) * | 2019-12-30 | 2020-03-31 | 嘉兴怡萃生物科技有限公司 | Efficient and comprehensive extraction method of effective components in amber |
| CN111424067A (en) * | 2020-06-02 | 2020-07-17 | 好当家集团有限公司 | Method for extracting low-component sea cucumber bioactive peptide |
| CN113521796A (en) * | 2021-06-10 | 2021-10-22 | 江苏高科制药设备有限公司 | Air-lift adsorption type supercritical extraction pharmaceutical system |
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| CN113521796A (en) * | 2021-06-10 | 2021-10-22 | 江苏高科制药设备有限公司 | Air-lift adsorption type supercritical extraction pharmaceutical system |
| CN113521796B (en) * | 2021-06-10 | 2022-05-27 | 江苏高科制药设备有限公司 | Air-lift adsorption type supercritical extraction pharmaceutical system |
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Application publication date: 20190920 |