CN107082820A - A kind of method that pulsating negative pressure low temperature extracts lentinan - Google Patents
A kind of method that pulsating negative pressure low temperature extracts lentinan Download PDFInfo
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- CN107082820A CN107082820A CN201710276706.4A CN201710276706A CN107082820A CN 107082820 A CN107082820 A CN 107082820A CN 201710276706 A CN201710276706 A CN 201710276706A CN 107082820 A CN107082820 A CN 107082820A
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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 method that pulsating negative pressure low temperature extracts lentinan, comprise the following steps：Fresh mushroom raw material is added water mashing, mushroom slurries are obtained；Or by fresh mushroom raw material drying, crush, obtain dried thin mushroom powder, dried thin mushroom powder added water mixing, mushroom slurries are obtained；Mushroom slurries are extracted under conditions of shear agitation, Extracting temperature is not higher than 50 DEG C, extract pressure and use pulsating negative pressure；After extraction terminates, separation of solid and liquid obtains filter residue and extract solution；Extract solution is concentrated, and uses ethanol precipitation, precipitation is further dried, produced.Pollution The present invention reduces the wasting of resources and to environment, add the added value of mushroom, promote the dissolution of lentinan using mechanical shearing and negative pressure cavitation double action, improve the yield of lentinan, there is with low cost, environmentally friendly, simple to operate, safety, the energy is saved.
Description
Technical field
The invention belongs to technical field of polysaccharide extraction, and in particular to a kind of pulsating negative pressure low temperature extracts the side of lentinan
Method.
Background technology
Mushroom delicious flavour, fragrance make people mentally refreshing is nutritious, not only containing multiple nutritional components such as polysaccharide, cellulose, amino
Acid, cartinellin, lenthionine and mineral matter element iron, calcium, phosphorus etc., also containing abundant provitamin D.Mushroom has fine
Immunization, it can improve body's immunity, anti-aging, cancer-resisting, lowering blood pressure and blood fat, norcholesterol, separately
Outer mushroom also plays therapeutic action to diabetes, pulmonary tuberculosis, catarrhal jaundice, neuritis etc., and indigestion, constipation are can be used for again
Deng, and the performance of these effects is all closely related with its polysaccharide.
But it is high that mushroom belongs to water content（Typically 90% or so）Rotten, fresh-keeping difficult food materials are easy to, must be as early as possible after adopting
Marketing fresh or processing, otherwise product will lose commodity value quickly.In addition, in mushroom machining and shaping trimming technique, producing a large amount of
Mushroom handle, inferior mushroom etc., except it is a small amount of be processed into the products such as mushroom sauce, mushroom pine in addition to, largely go out of use, discarded mushroom mushroom
Handle, inferior mushroom etc. are at least the 1/10~1/8 of its yield, and it is all directly discarded or inexpensively handled by most producer, is not only caused
The great wasting of resources, is also polluted to environment.If the active ingredients such as polysaccharide contained therein are carried out fully effectively sharp
With, the added value of product of mushroom can be not only improved, mushroom processed output is improved, while the discharge capacity of discarded object can be also reduced, tool
There is good economy and environmental benefit.
Lentinan is that obtained effective active composition is extracted from mushroom, is the principle active component of mushroom.It is right at present
Hot water and dilute alkaline soln being used the extraction of lentinan, the Chinese patent of Application No. 201410700171.5 discloses one kind more
The method of semi-bionic extraction method lentinan, is mainly comprised the following steps：Pretreatment of raw material, slightly acidic water are extracted, alkalescent water is extracted, neutral
Water extracts, prepares eluent, prepare trapped fluid, be concentrated under reduced pressure, centrifuge removal precipitum, precipitation vacuum drying and crushing packing；
Although this method extract yield is high, it is long to there is extraction time, and easily causing glycosidic bond fracture and conformation change in polysaccharide influences it
Activity.In addition, also there is the report extracted using ultrasonic wave, microwave etc. to lentinan, although extraction time shortens, but sets
Standby cost is higher, limits its application industrially.
The content of the invention
Based on the deficiencies in the prior art, lentinan is extracted it is an object of the invention to provide a kind of pulsating negative pressure low temperature
Method, uses fresh or dried mushroom for raw material, the method being combined through mechanical shearing broken wall and negative pressure cavitation broken wall,
Polysaccharide is extracted at a temperature of not higher than 50 DEG C, sporoderm-broken rate can be not only improved, promotes the dissolution of polysaccharide, polysaccharide yield is improved,
Extraction time can be shortened again, energy resource consumption is reduced, its physiologically active is kept to greatest extent.
To achieve these goals, the technical solution adopted by the present invention is：
A kind of method that pulsating negative pressure low temperature extracts lentinan, comprises the following steps：
（1）Fresh mushroom raw material is added water mashing, mushroom slurries are obtained；Or by fresh mushroom raw material drying, crushing, obtain dried thin mushroom
Powder, dried thin mushroom powder is added water mixing, mushroom slurries are obtained；
（2）Mushroom slurries are extracted under conditions of shear agitation, Extracting temperature is not higher than 50 DEG C, extract pressure and use arteries and veins
Rush negative pressure；After extraction terminates, separation of solid and liquid obtains filter residue and extract solution；
（3）By step（2）Gained extract solution is concentrated, and uses ethanol precipitation, and precipitation is further dried, produced.
Preferably, step（1）It is middle by fresh mushroom raw material add water mashing when, the mass ratio of fresh mushroom raw material and water is 1：5~8.
Further, step（2）Described in shear agitation rotating speed be 5000 ~ 10000 revs/min.
Preferably, step（1）Middle dried thin mushroom powder add water mixing when, the mass ratio of dried thin mushroom powder and water is 1：8~10.
Further, step（2）Described in shear agitation rotating speed be 200 ~ 500 revs/min.
Preferably, step（2）Described in pulsating negative pressure be negative pressure-normal pressure be alternatively formed pulsed circulation, concrete operations
For：- 93 ~ -97 kPa are evacuated to, after being kept for 1 ~ 2 minute, recovers to normal pressure, is circulated 3 ~ 5 times with this.
Preferably, step（3）Described in dry using vacuum drying（The kPa of vacuum -80 ~ -98,40 ~ 60 DEG C of temperature）Or
Freeze-drying.
In the above method fresh mushroom raw material used refer to the quality xianggu after cleaning, etc. outer mushroom and incompleteness mushroom（Such as mushroom
Lid, mushroom handle）One or both of it is mixed above, the dried thin mushroom powder by fresh mushroom raw material drying, crush and obtain, can also adopt
Directly crushed and be made with common commercially available dried thin mushroom on the market.
The present invention reduces because（Mushroom raw material）The wasting of resources caused not in time and the pollution to environment are handled, is expanded
The application of product, adds the added value of mushroom, improves plantation unit and the economic benefit of peasant household；The present invention is using machinery
The method that shearing broken wall is combined with negative pressure cavitation broken wall, can not only improve sporoderm-broken rate, promote object（Lentinan）'s
Dissolution, improves the yield of object, can also shorten broken wall extraction time, improves extracting efficiency；The present invention is no more than 50 DEG C
At a temperature of extracted, not only can shorten the heat time, can also reduce due to when high temperature is long extraction to object structural damage,
Keep the physiologically active of object.In a word, the method for the invention has with low cost, environmentally friendly, simple to operate, safety, saving
The advantages of energy.
Brief description of the drawings
Fig. 1 is the structural representation of the extraction element；
Fig. 2 is the structural representation of kuppe in Fig. 1.
Embodiment
In order that the technical purpose of the present invention, technical scheme and beneficial effect are clearer, with reference to specific embodiment
Technical scheme is further illustrated, but the embodiment is intended to explain the present invention, and it is not intended that right
The limitation of the present invention, in the examples where no specific technique or condition is specified, according to the technology described by document in the art or
Condition is carried out according to product description.
Extraction element used in following embodiments, such as Fig. 1 and Fig. 2, including tank body 10, upper lid 5 and rabbling mechanism.On described
Lid 5 is installed on the vacuum meter 6 being provided with the upper port of tank body 10, upper lid 5 for detecting vacuum in tank body 10, upper lid 5
Air inlet and bleeding point are additionally provided with the form 4 of situation in tank body 10, upper lid 5 provided with handle 22 and for observing, it is described enter
Gas port is communicated with admission line 3, and admission line 3, which is provided with, to be used to control the opening/closing intake valve 2 of air inlet, and bleeding point is communicated with
Pump-line, pump-line is communicated with vacuum tank provided with the opening/closing extraction valve 7 of control bleeding point, the other end of pump-line
19, the vavuum pump 17 for vacuumizing, and the pipe between vacuum tank 19 and vavuum pump 17 are connected with by pipeline on vacuum tank 19
Road is provided with vacuum valve 18.The side wall on the top of tank body 10 is provided with charging aperture, and charging aperture is communicated with feed pipe 8, feeds
Pipeline 8, which is provided with, to be used to control the opening/closing inlet valve 9 of charging aperture；The madial wall of the bottom of tank body 10 was provided with for adding for heating
Heat pipe 16, the bottom of tank body 10 is provided with the thermometer 14 for detecting temperature in tank body 10；The bottom surface of tank body 10 is in convex downwards
Sphere, the center of the bottom surface of tank body 10 is provided with discharging opening, and discharging opening is communicated with discharge pipe 20, and discharge pipe 20 is provided with using
In the opening/closing outlet valve 21 of control discharging opening.Bottom in tank body 10 is provided with kuppe 13, and whirlpool is formed during in favor of shear agitation
Negative pressure is flowed, material is sucked into broken material in kuppe 13；The kuppe 13 includes tubular case 131, and case 131
The longitudinal center line of longitudinal center line and tank body 10 coincide, along the circumferential direction uniform intervals are provided with some circles on case 131
Hole 132, the upper end of case 131 is fixed with some connecting rods 12, and the kuppe 13 is fixed by connecting rod 12 and tank body 10 to be connected
Connect.The rabbling mechanism includes agitating shaft 11, and the longitudinal center line of the agitating shaft 11 is mutually overlapping with the longitudinal center line of tank body 10
Close, the upper end of agitating shaft 11 is provided with through and out the end of the agitating shaft 11 of lid 5 on upper lid 5, and stretching to be stirred for driving
The adjustable speed motor 1 of the rotation of axle 11 is mixed, the lower end of agitating shaft 11 extends to the bottom of kuppe 13, and the bottom of agitating shaft 11
Shearing cutter head 15 is installed.
Wherein, the heating tube 16 is electrothermal tube or steam(-)coil, and is connected with temperature sensor.The vacuum tank
19 volumes are more than 3 times of the volume of tank body 10, and moment in tank body 10 can be made to reach required negative pressure.In use, according to mesh in material
Nutritional ingredient and functional active components are marked, when being extracted, non-heated may be selected（Normal temperature）Extract or heat（Not higher than 50
℃）Extract.
When non-heated is extracted, upper lid 5 is opened first with handle 22, intake valve 2, extraction valve 7, inlet valve 9 is closed and goes out
Expect valve 21, open vavuum pump 17 and vacuum valve 18, make to be in certain vacuum state in vacuum tank 19；By material and Extraction solvent
（Water）Add in tank body 10, or material is added in tank body 10, cover after lid 5, open adjustable speed motor 1, make agitating shaft 11
Drive shearing cutter head 15 to operate, open extraction valve 7, moment in tank body 10 is formed vacuum state, then open inlet valve 9, profit
With negative pressure by Extraction solvent（Water）It is pumped into tank body 10, closes inlet valve 9；Negative-pressure vacuum state is now in tank body 10, is protected
The vacuum 1 ~ 2 min is held, extraction valve 7 is then shut off and opens the releasing negative pressure of intake valve 2, after the reading of vacuum meter 6 is 0, close
Intake valve 2 is closed, extraction valve 7 is again turned on, makes tank body 10 connect to form negative pressure with vacuum tank 19, so repeatedly 3~5 times,
Outlet valve 21 is opened, material extract solution is released, that is, completes an extraction process.
During heating extraction, upper lid 5 is opened first with handle 22, intake valve 2, extraction valve 7, inlet valve 9 and discharging is closed
Valve 21, opens vavuum pump 17 and vacuum valve 18, makes to be in certain vacuum state in vacuum tank 19；By Extraction solvent（Water）Add
In tank body 10, or lid 5 is covered, open adjustable speed motor 1, make agitating shaft 11 drive shearing cutter head 15 to operate, open extraction valve
7, moment is formed vacuum state, then open inlet valve 9, using negative pressure by Extraction solvent（Water）It is pumped into tank body 10
It is interior, inlet valve 9 and extraction valve 7 are closed, lid 5 is then covered, heating tube 16 is opened and is heated, after design temperature to be achieved,
Lid 5 in opening, material is put into tank body 10, covers lid 5；Adjustable speed motor 1 is opened, agitating shaft 11 is driven shearing cutter head
15 operatings, open extraction valve 7, moment in tank body 10 is formed vacuum state, keep the vacuum 1 ~ 2 min, be then shut off taking out
Air valve 7 simultaneously opens the releasing negative pressure of intake valve 2, after the reading of vacuum meter 6 is 0, closes intake valve 2, is again turned on extraction valve 7, makes
Tank body 10 connects to form negative pressure with vacuum tank 19, so repeatedly 3~5 times, opens outlet valve 21, material extract solution is put
Go out, that is, complete an extraction process.
Embodiment 1
A kind of method that pulsating negative pressure low temperature extracts lentinan, comprises the following steps：
（1）By the fresh mushroom raw material and water after cleaning according to mass ratio 1：5 are put into extraction element, with 5000 revs/min of rotating speed
Shear agitation is beaten, and obtains mushroom slurries；
（2）By mushroom slurries in shear agitation（5000 revs/min of rotating speed）Under conditions of extracted, be evacuated to -95 kPa,
After being kept for 2 minutes, recover to normal pressure, circulated 4 times with this, centrifugation obtains material residue and supernatant；By material residue shear agitation bar
Extracted under part, be evacuated to -95 kPa, after being kept for 2 minutes, recovered to normal pressure, circulated 3 times, after centrifugation, obtained with this
To filter residue and filtrate, merging filtrate and supernatant obtain extract solution；
（3）By step（2）Gained extract solution is concentrated under reduced pressure（45~50 DEG C of the kPa of vacuum -98, temperature）To original volume 1/2 ~
1/3, add the ethanol of 3 times of volumes and take precipitation to be dried in vacuo after lentinan, centrifugation to precipitate（The kPa of vacuum -80 ~ -98, temperature
40 ~ 60 DEG C of degree）, produce.
Embodiment 2
A kind of method that pulsating negative pressure low temperature extracts lentinan, comprises the following steps：
（1）By the fresh mushroom raw material and water after cleaning according to mass ratio 1：8 are put into extraction element, 50 DEG C are heated to, with 10000
Rev/min rotating speed cutting stirring be beaten, obtain mushroom slurries；
（2）By mushroom slurries in shear agitation（10000 revs/min of rotating speed）Under conditions of extracted, be evacuated to -93
KPa, after being kept for 2 minutes, is recovered to normal pressure, is circulated 5 times with this, centrifugation obtains material residue and supernatant；By material residue in shear agitation
Under conditions of extracted, be evacuated to -93 kPa, after being kept for 2 minutes, recover to normal pressure, circulated 5 times with this, centrifuge
Afterwards, filter residue and filtrate, merging filtrate and supernatant are obtained, extract solution is obtained；
（3）By step（2）Gained extract solution is concentrated under reduced pressure（45~50 DEG C of the kPa of vacuum -98, temperature）To original volume 1/2 ~
1/3, add the ethanol of 3 times of volumes and take precipitation to be dried in vacuo after lentinan, centrifugation to precipitate（The kPa of vacuum -80 ~ -98, temperature
40 ~ 60 DEG C of degree）, produce.
Embodiment 3
A kind of method that pulsating negative pressure low temperature extracts lentinan, comprises the following steps：
（1）By fresh mushroom raw material drying, crushing, 40 mesh sieves are crossed, dried thin mushroom powder are obtained, by dried thin mushroom powder and water according to mass ratio 1：
10 are put into extraction element, are heated to 50 DEG C, are stirred with 500 revs/min of rotating speed cutting, obtain mushroom slurries；
（2）By mushroom slurries in shear agitation（500 revs/min of rotating speed）Under conditions of extracted, be evacuated to -97 kPa,
After being kept for 1 minute, recover to normal pressure, circulated 3 times with this, centrifugation obtains material residue and supernatant；By material residue shear agitation bar
Extracted under part, be evacuated to -97 kPa, after being kept for 1 minute, recovered to normal pressure, circulated 2 times, after centrifugation, obtained with this
To filter residue and filtrate, merging filtrate and supernatant obtain extract solution；
（3）By step（2）Gained extract solution is concentrated under reduced pressure（45~50 DEG C of the kPa of vacuum -98, temperature）To original volume 1/2 ~
1/3, add the ethanol of 3 times of volumes and take precipitation to be dried in vacuo after lentinan, centrifugation to precipitate（The kPa of vacuum -80 ~ -98, temperature
40 ~ 60 DEG C of degree）, produce.
Embodiment 4
A kind of method that pulsating negative pressure low temperature extracts lentinan, comprises the following steps：
（1）By fresh mushroom raw material drying, crushing, 40 mesh sieves are crossed, dried thin mushroom powder are obtained, by dried thin mushroom powder and water according to mass ratio 1：
8 are put into extraction element, are stirred with 200 revs/min of rotating speed cutting, obtain mushroom slurries；
（2）By mushroom slurries in shear agitation（200 revs/min of rotating speed）Under conditions of extracted, be evacuated to -95 kPa,
After being kept for 2 minutes, recover to normal pressure, circulated 4 times with this, centrifugation obtains material residue and supernatant；By material residue shear agitation bar
Extracted under part, be evacuated to -95 kPa, after being kept for 2 minutes, recovered to normal pressure, circulated 3 times, after centrifugation, obtained with this
To filter residue and filtrate, merging filtrate and supernatant obtain extract solution；
（3）By step（2）Gained extract solution is concentrated under reduced pressure（45~50 DEG C of the kPa of vacuum -98, temperature）To original volume 1/2 ~
1/3, add the ethanol of 3 times of volumes and take precipitation to be dried in vacuo after lentinan, centrifugation to precipitate（The kPa of vacuum -80 ~ -98, temperature
40 ~ 60 DEG C of degree）, produce.
Through measurement, the lentinan yield of embodiment 1 is 71.34 g/kg, and the lentinan yield of embodiment 2 is 100.42 g/
Kg, the lentinan yield of embodiment 3 is 95.65 g/kg, and the lentinan yield of embodiment 4 is 88.67g/kg；Fresh mushroom is former
Material is extracted according to conventional hot water（90 DEG C of 3 h of extraction）, lentinan yield is 35.13 g/kg, the extraction time of embodiment 1 ~ 4
It is far smaller than the time of conventional hot water's extraction, but the lentinan yield of embodiment 1 ~ 4 is respectively that hot water extraction's lentinan is obtained
2.03 times, 2.86 times, 2.72 times, 2.52 times of rate.
Claims (7)
1. a kind of method that pulsating negative pressure low temperature extracts lentinan, it is characterised in that comprise the following steps：
（1）Fresh mushroom raw material is added water mashing, mushroom slurries are obtained；Or by fresh mushroom raw material drying, crushing, obtain dried thin mushroom
Powder, dried thin mushroom powder is added water mixing, mushroom slurries are obtained；
（2）Mushroom slurries are extracted under conditions of shear agitation, Extracting temperature is not higher than 50 DEG C, extract pressure and use arteries and veins
Rush negative pressure；After extraction terminates, separation of solid and liquid obtains filter residue and extract solution；
（3）By step（2）Gained extract solution is concentrated, and uses ethanol precipitation, and precipitation is further dried, produced.
2. the method that pulsating negative pressure low temperature extracts lentinan according to claim 1, it is characterised in that：Step（1）It is middle to incite somebody to action
Fresh mushroom raw material add water mashing when, the mass ratio of fresh mushroom raw material and water is 1：5~8.
3. the method that pulsating negative pressure low temperature extracts lentinan according to claim 2, it is characterised in that：Step（2）Middle institute
The rotating speed for stating shear agitation is 5000 ~ 10000 revs/min.
4. the method that pulsating negative pressure low temperature extracts lentinan according to claim 1, it is characterised in that：Step（1）In do
Mushroom powder add water mixing when, the mass ratio of dried thin mushroom powder and water is 1：8~10.
5. the method that pulsating negative pressure low temperature extracts lentinan according to claim 4, it is characterised in that：Step（2）Middle institute
The rotating speed for stating shear agitation is 200 ~ 500 revs/min.
6. the method that lentinan is extracted according to any pulsating negative pressure low temperature of claim 1 to 5, it is characterised in that step
（2）Described in pulsating negative pressure be pulsed circulation that negative pressure-normal pressure is alternatively formed, concrete operations are：It is evacuated to -93 ~ -97
KPa, after being kept for 1 ~ 2 minute, is recovered to normal pressure, is circulated 3 ~ 5 times with this.
7. the method that lentinan is extracted according to any pulsating negative pressure low temperature of claim 1 to 5, it is characterised in that：Step
（3）Described in dry using vacuum drying or be freeze-dried.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110760369A (en) * | 2019-11-08 | 2020-02-07 | 润科生物工程（福建）有限公司 | Method for purely physically extracting arachidonic acid oil |
| CN111087485A (en) * | 2019-10-31 | 2020-05-01 | 华南理工大学 | Method for preparing noni polysaccharide with high anticancer and antioxidant activity by using gradient physical field |
| CN111743816A (en) * | 2019-03-29 | 2020-10-09 | 北京东方淼森生物科技有限公司 | Skin care product additive with anti-haze effect and industrial preparation method thereof |
| CN114685691A (en) * | 2022-04-19 | 2022-07-01 | 河南工业大学 | Low-temperature preparation method of lentinan powder |
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| CN101555292A (en) * | 2009-05-26 | 2009-10-14 | 何颖娜 | Method for extracting lentinan from foot of lentinus edodes |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111743816A (en) * | 2019-03-29 | 2020-10-09 | 北京东方淼森生物科技有限公司 | Skin care product additive with anti-haze effect and industrial preparation method thereof |
| CN111087485A (en) * | 2019-10-31 | 2020-05-01 | 华南理工大学 | Method for preparing noni polysaccharide with high anticancer and antioxidant activity by using gradient physical field |
| CN110760369A (en) * | 2019-11-08 | 2020-02-07 | 润科生物工程（福建）有限公司 | Method for purely physically extracting arachidonic acid oil |
| CN114685691A (en) * | 2022-04-19 | 2022-07-01 | 河南工业大学 | Low-temperature preparation method of lentinan powder |
| CN114685691B (en) * | 2022-04-19 | 2024-05-03 | 河南工业大学 | Low-temperature preparation method of lentinan polysaccharide powder |
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