CN104231281B - A kind of method extracting separation gutta-percha - Google Patents
A kind of method extracting separation gutta-percha Download PDFInfo
- Publication number
- CN104231281B CN104231281B CN201410500227.2A CN201410500227A CN104231281B CN 104231281 B CN104231281 B CN 104231281B CN 201410500227 A CN201410500227 A CN 201410500227A CN 104231281 B CN104231281 B CN 104231281B
- Authority
- CN
- China
- Prior art keywords
- gutta
- percha
- steam explosion
- treatment
- eucommia bark
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of method extracted and separate gutta-percha, including pre-treatment, pretreatment, alkali process, enzymolysis and extraction purification step, its innovative point is: after pre-treatment step, also include steam explosion pre-treatment step, material after pre-treatment is placed in the water of 20～30 DEG C immersion 0～24h, and the material after then soaking is put into steam blasting device and is carried out steam explosion.The present invention utilizes steam explosion to extract and separates gutta-percha, Cortex Eucommiae raw material need not be carried out over grind, extraction disengaging time is short, effectively prevent because lengthy fermentation causes part gutta-percha oxidized, the filament gutta-percha of ecosystem can be obtained, maintain the biological nature of colloid, physical property and physical state, keep original molecular structure and the degree of polymerization.It addition, the present invention is while utilizing steam explosion pretreatment to extract separation gutta-percha, utilizes membrance concentration and isolation technics, it is thus achieved that eucommia bark polycose, improve value-added content of product.
Description
Technical field:
The invention belongs to natural product Gutta extraction separation field, specifically, one utilizes steam quick-fried
The method separating gutta-percha is extracted in broken method pretreatment from the Cortex Eucommiae.
Background technology:
The Cortex Eucommiae (Eucommia ulmoides Oliv.) is the distinctive famous and precious woody medicinal species of China, is referred to as
" living fossil plant ", is also the Relict Plant in the Tertiary Period existing only in China, be distributed in more than 20 province in the whole nation (city,
Autonomous region), be predominantly located at sweet, Shan, Shanxi, Henan, Hunan, Hubei Province, river, Yunnan, Guizhou Province, osmanthus, Jiangxi, Fujian etc. save,
Municipal Plain is to the hills of height above sea level 1690 meters and mountain region, and Natural Central is in Central Region.20th century
Since the eighties, under the ever-increasing promotion of natural rubber demand, the exploitation of gutta-percha is as adjusting rubber
The Important Action of the industrial structure, the succedaneum gutta-percha of various places active development natural rubber, promote the cultivation of the Cortex Eucommiae
Training area drastically expands, and the cultivated area of current China Cortex Eucommiae has evolved to about 350,000 hectares, accounts for world's Cortex Eucommiae
More than the 99% of total amount.Gutta-percha is present in the white filament in each organ Gutta_containing cell of the Cortex Eucommiae, it
It it is (trans-polyisoprene) a kind of special natural macromolecular material.Along with natural gutta-percha is changed into
The success of trans-polyisoprene vulcanite so that it is there is thermoplasticity, insulating properties, resistance to water, acidproof
The features such as alkalescence, will have in various fields and be worth widely.But the output capacity of gutta-percha is low and extracts
The features such as the complication of journey, production cost height and environmental pollution are serious, limit its industrialized production.
The at present research of gutta-percha and application aspect, major part research concentrate on the primary modified of gutta-percha or
Directly utilizing, such as additive, blend components etc., the exploitation of single gutta-percha, cost is high, and difficulty is big,
High-valued gutta-percha product is little, and gutta-percha low cost utilization power is the most pessimistic.At present, gutta-percha
Extracting method such as high speed water conservancy to stir the method for washing (Chinese patent 86100216) disclosed, the prior fermentation cycle is long
Reach one month, process with NaOH aqueous solution steaming and decocting the most again.The NaOH consumption that this method expends is too big, productivity
Low, the purity of gained glue is the highest.And solvent extraction method, such as the extracting method of patent ZL00135831.6,
Mostly being the solvent by low polarity, chloroform, low boiling petroleum ether, benzene class is extracted, and makes gutta-percha from plant
Cell is dissolved out, then through adding methanol, ethanol, acetone, ethyl acetate polar solvent makes colloid
Separate out.The microbial method (Chinese patent: CN101914211A) comparatively cleaned extracts gutta-percha,
Shortcoming is that the cycle is long, and cost is high, and its gutta-percha structure change in very long sweat is serious, and oxidation becomes
Matter, molecular weight diminishes, and impurity content is many, has a strong impact on its later use.There is following being difficult in said method
The shortcoming overcome: the most directly extracting with Cortex Eucommiae raw material, organic solvent consumption is big, and environmental pollution is serious.
If 2. raw material pulverizing is abundant not, colloid can not leach completely, and productivity is affected.3. Cortex Eucommiae material
After pulverizing, reduce the elasticity of gutta-percha, toughness, tensile strength.The ecosystem of high polymerization degree can not be obtained
Gutta-percha.4. equipment investment is big, and production cost remains high.Therefore, new Cortex Eucommiae biorefinery is developed
Pretreatment mode and gutta-percha separation method based on biorefinery are most important.
Because the above-mentioned existing Cortex Eucommiae extracts the defect that the method separated exists, the present inventor is based on being engaged in this
Series products manufactures and designs for many years abundant practical experience and Professional knowledge, and coordinates the utilization of scientific principle, actively adds
With research and innovation, to founding a kind of method utilizing steam explosion pretreatment to extract separation gutta-percha, profit
Extract the gutta-percha separated by the method, greatly reduce the extraction cost of gutta-percha, general existing by improving
Some Apparatus and method fors so that it is have more practicality.Through constantly research, design, and through repeatedly trying
After making sample and improving, finally create the present invention having practical value.
Summary of the invention:
It is an object of the invention to provide a kind of side utilizing steam explosion pretreatment to extract separation gutta-percha
Method, it is possible to obtain the filament gutta-percha of ecosystem.
For solving above-mentioned technical problem, the present invention adopts the following technical scheme that realization: a kind of extraction separates the Cortex Eucommiae
The method of glue, including pre-treatment, alkali process, enzymolysis and extraction purification step, its innovative point is: front
After processing step, also include steam explosion pre-treatment step, the material after pre-treatment is placed on 20～30 DEG C
Water in soak 0～24h, the material after then soaking is put into steam blasting device and is carried out steam explosion.
Further, the described method extracting separation gutta-percha comprises the following steps:
(1) pre-treatment: by Cortex Eucommiae raw material, roguing processes, and being crushed to particle diameter is 1～15cm, is placed in dry
Dry shady and cool at standby；
(2) steam explosion pretreatment: the material after pre-treatment is placed in the water of 20～30 DEG C immersion 0～
24h, the material after then soaking puts into steam blasting device and carries out steam explosion, the pressure of steam explosion
Being 0.5～1.8MPa, temperature when controlling the steam explosion of steam blasting device is 140～180 DEG C, and ties up
Pressure 1～15min, after steam explosion, temperature of charge is room temperature；
(3) alkali processes: uses NaOH solution to extract twice the filtering residue of step (2), merges twice filter
Liquid, salt acid for adjusting pH to 5.5～6.0, concentrated solution is poured in ethanol solution after concentrating by wound membrane, separates out Du
Secondary polysaccharide, filters, and separates eucommia bark polycose, is dried, obtains finished product eucommia bark polycose；
(4) enzymolysis: the filtering residue in step (3) is added distilled water, with vinegar acid for adjusting pH to 4.8～5.2,
After being subsequently adding combinative enzyme hydrolysis, rinse lignin residue, obtain the thick glue of the Cortex Eucommiae；
(5) extraction purification: mix with petroleum ether after the Cortex Eucommiae thick glue dried that step (4) is obtained,
Condensation is extracted, heat filtering remove impurity, filtrate cold preservation, separates out gutta-percha, reclaims petroleum ether, is vacuum dried
To eucommia ulmoides refined glue.
Further, described step (3) is particularly as follows: by the filtering residue and 0.5～the NaOH of 4% of step (2)
Solution, according to the ratio mixing that solid-liquid ratio is 1:5～1:20, extracts 1～3h under the conditions of 60～80 DEG C,
After filtration, pump to receiver, during second extraction, mix according to the solid-liquid ratio of 1:5～1:15, extract temperature
Spend identical with first time with the time, separating filtrate, filtering residue stores for future use, after merging twice filtrate, with 4～
The salt acid for adjusting pH 5.5～6.0 of 8mol/L, utilizes the wound membrane being 300D by molecular weight to concentrate, outlet pressure
Power 0.2～0.3Mpa, until after concentrated solution density is 1.10～1.15g/mL, then concentrated solution is poured into 2～3
In the ethanol solution of times volume 95%, separate out eucommia bark polycose, the method separating polyose that application periosteum filters, its
Middle periosteum molecular cut off 1000～5000D, utilizes the method for vacuum lyophilization to be dried, i.e. obtains finished product
Eucommia bark polycose.
Further, described eucommia bark polycose mainly includes rhamnosan >=1.66%, arabinan
>=6.72%, mannan >=4.11%, glucosan >=6.42%, xylan >=4.75%, glucuronic acid >=1.65%.
Further, described step (4) particularly as follows: by the filtering residue of step (3) according to solid-liquid ratio 1:10～
The ratio of 1:40 adds distilled water, regulates pH to 4.8～5.2 with sodium acetate, is subsequently adding 30～100IU/g
Compound enzyme, under the conditions of 48～52 DEG C, after combinative enzyme hydrolysis 36～84h, utilize high-pressure cleaning device to rush
Wash lignin residue, hydraulic pressure 100bar～800bar, obtain the thick glue of the Cortex Eucommiae.
Further, described compound enzyme mainly includes pectase 18000IU/g, xylanase 3500IU/g,
Cellulase 5500IU/g and 1,4 beta-glucanase >=11000IU/g.
Further, described step (5) is particularly as follows: the thick glue of Cortex Eucommiae step (4) obtained is done
After dry process, according to ratio and petroleum ether (boiling range: the 60～90 DEG C) mixing of solid-liquid ratio 1:5～1:20,
Under the conditions of 80～85 DEG C, condensation extracts 1～4h, and heat filtering goes the removal of impurity, by liquid-4～-20 DEG C of cold preservations
0.5～3h, after gutta-percha separates out, reclaim petroleum ether, i.e. obtain eucommia ulmoides refined glue through vacuum drying.
The effect of the present invention:
1, the present invention utilizes steam explosion to extract and separates gutta-percha, Cortex Eucommiae need not be carried out over grind,
Extraction disengaging time is short, effectively prevent owing to lengthy fermentation causes part gutta-percha oxidized, can obtain
Obtain the filament gutta-percha of ecosystem, maintain the biological nature of colloid, physical property and physical state, keep
Original molecular structure and the degree of polymerization.
2, the present invention utilizes eucommia bark for raw material, extracts eucommia bark polycose and gutta-percha continuously, introduces film skill
The operations such as art carries out separating, concentration, can improve quality and the yield of eucommia bark polycose, and filtering and impurity removing is abundant, institute
Take time short, extract separation temperature low.
3, the present invention extracts the extract residue after eucommia bark polycose, extracts gutta-percha through enzyme hydrolysis, greatly
Reducing greatly the extraction cost of gutta-percha, processing step is few, and equipment is simple, easy to operate, has production week
Phase is short, pollutes little, the industrialized production of the advantages, beneficially gutta-percha such as production cost is low.
4, the present invention is while extracting separation gutta-percha, it is thus achieved that eucommia bark polycose, improves the attached of product
Value added, reduce the Cost Problems during Gutta extraction, develop gutta-percha based on biorefinery high
Value extraction separation method.
Accompanying drawing illustrates:
Fig. 1 is that in the embodiment of the present invention, the method schematic diagram separating gutta-percha is extracted in steam explosion pretreatment.
Detailed description of the invention:
With specific embodiment, technical scheme is elaborated below in conjunction with the accompanying drawings.
The a kind of of the present invention extracts the method separating gutta-percha, including pre-treatment, alkali process, enzymolysis and extraction
Purification step, after pre-treatment step, also includes steam explosion pre-treatment step, by the material after pre-treatment
Being placed in the water of 20～30 DEG C immersion 0～24h, the material after then soaking is put into steam blasting device and is entered
Row steam explosion.
Embodiment 1:
A kind of method extracting separation gutta-percha, comprises the steps:
(1) pre-treatment: by eucommia bark, after roguing processes, according to the prescription of Chinese Pharmacopoeia,
Qualified through inspection, dry eucommia bark machinery suitably to be pulverized, granularity is 1cm, is placed in dry
At Yin Liang standby；
(2) steam explosion: the material handled well in step (1) is put into steam blasting device and carries out steam
Explosion, the pressure of steam explosion is 0.5MPa, and temperature when controlling the steam explosion of steam blasting device is
140 DEG C, and tie up pressure 15min, after steam explosion, temperature of charge is room temperature；
(3) by the filtering residue in step (2) and the NaOH solution of 0.5%, according to the ratio that solid-liquid ratio is 1:5
Example mixes, and extracts 3h under the conditions of 60 DEG C, and after filtration, pump to receiver, during second extraction, according to 1:15
Solid-liquid ratio mixing, Extracting temperature is identical with first time with the time, separating filtrate, and filtering residue stores for future use, conjunction
And after twice filtrate, with the salt acid for adjusting pH 5.5 of 4mol/L, utilize the wound membrane being 300D by molecular weight
Concentrate, outlet pressure 0.2Mpa, until after concentrated solution density is 1.10g/mL, then pour concentrated solution into 2
In the ethanol solution of times volume 95%, after eucommia bark polycose separates out, the method separating polyose that application periosteum filters,
Wherein periosteum molecular cut off 1000D, polysaccharide utilizes the method for vacuum lyophilization to be dried, i.e. obtains finished product
Eucommia bark polycose；
(4) enzymolysis: the filtering residue in step (3) is added distilled water according to the ratio of solid-liquid ratio 1:10,
Regulating pH to 4.8 with sodium acetate, be subsequently adding the compound enzyme of 30IU/g, compound enzyme mainly includes pectase
18000IU/g, xylanase 3500IU/g, cellulase 5500IU/g, 1,4 beta-glucanase >=11000IU/g
Composition, under the conditions of 48 DEG C, after hydrolysis 84h, utilizes high-pressure cleaning device to rinse lignin residue, hydraulic pressure
100bar, obtains the thick glue of the Cortex Eucommiae；
(5) extraction purification: after the thick glue of the Cortex Eucommiae in step (4) is dried process, according to solid-liquid ratio
The ratio of 1:5 and petroleum ether (boiling range: 60～90 DEG C) mixing, under the conditions of 80 DEG C, 4h, heat are extracted in condensation
The removal of impurity is gone in filtration, by liquid at-4 DEG C of cold preservation 3h, after gutta-percha separates out, reclaims petroleum ether, Jing Guozhen
Empty drying to obtain eucommia ulmoides refined glue.
Embodiment 2:
A kind of method extracting separation gutta-percha, comprises the steps:
(1) pre-treatment: by eucommia bark, after roguing processes, according to the prescription of Chinese Pharmacopoeia,
Qualified through inspection, dry eucommia bark machinery suitably to be pulverized, granularity is 10cm, is placed in dry
Dry shady and cool at standby；
(2) steam explosion: the material handled well in step (1) is put into steam blasting device and carries out steam
Explosion, the pressure of steam explosion is 1.2MPa, and temperature when controlling the steam explosion of steam blasting device is
160 DEG C, and tie up pressure 8min, after steam explosion, temperature of charge is room temperature；
(3) by the filtering residue in step (2) and the NaOH solution of 2%, according to the ratio that solid-liquid ratio is 1:10
Example mixes, and extracts 2h under the conditions of 70 DEG C, and after filtration, pump to receiver, during second extraction, according to 1:5
Solid-liquid ratio mixing, Extracting temperature is identical with first time with the time, separating filtrate, and filtering residue stores for future use, conjunction
And after twice filtrate, with the salt acid for adjusting pH 6 of 6mol/L, utilize the wound membrane being 300D by molecular weight
Concentrate, outlet pressure 0.2Mpa, until after concentrated solution density is 1.12g/mL, then pour concentrated solution into 2.5
In the ethanol solution of times volume 95%, after eucommia bark polycose separates out, the method separating polyose that application periosteum filters,
Wherein periosteum molecular cut off 3000D, polysaccharide utilizes the method for vacuum lyophilization to be dried, i.e. obtains finished product
Eucommia bark polycose；
(4) enzymolysis: the filtering residue in step (3) is added distilled water according to the ratio of solid-liquid ratio 1:25,
Regulating pH to 5.0 with sodium acetate, be subsequently adding the compound enzyme of 60IU/g, compound enzyme mainly includes pectase
18000IU/g, xylanase 3500IU/g, cellulase 5500IU/g, 1,4 beta-glucanase >=11000IU/g
Composition, under the conditions of 49 DEG C, after combinative enzyme hydrolysis 48h, utilizes high-pressure cleaning device to rinse lignin residue,
Hydraulic pressure 500bar, obtains the thick glue of the Cortex Eucommiae；
(5) extraction purification: after the thick glue of the Cortex Eucommiae in step (4) is dried process, according to solid-liquid ratio
The ratio of 1:10 and petroleum ether (boiling range: 60～90 DEG C) mixing, under the conditions of 83 DEG C, 2.5h is extracted in condensation,
Heat filtering goes the removal of impurity, by liquid at-10 DEG C of cold preservation 2h, after gutta-percha separates out, reclaims petroleum ether, warp
Cross vacuum drying and i.e. obtain eucommia ulmoides refined glue.
Embodiment 3:
A kind of method extracting separation gutta-percha, comprises the steps:
(1) pre-treatment: by eucommia bark, after roguing processes, according to the prescription of Chinese Pharmacopoeia,
Qualified through inspection, dry eucommia bark machinery suitably to be pulverized, granularity is 5cm, is placed in dry
At Yin Liang standby；
(2) steam explosion: the material handled well in step (1) is put into steam blasting device and carries out steam
Explosion, the pressure of steam explosion is 1.8MPa, and temperature when controlling the steam explosion of steam blasting device is
180 DEG C, and tie up pressure 1min, after steam explosion, temperature of charge is room temperature；
(3) by the filtering residue in step (2) and the NaOH solution of 4%, according to the ratio that solid-liquid ratio is 1:20
Example mixes, and extracts 1h under the conditions of 80 DEG C, and after filtration, pump to receiver, during second extraction, according to 1:10
Solid-liquid ratio mixing, Extracting temperature is identical with first time with the time, separating filtrate, and filtering residue stores for future use, conjunction
And after twice filtrate, with the salt acid for adjusting pH 6.0 of 8mol/L, utilize the wound membrane being 300D by molecular weight
Concentrate, outlet pressure 0.3Mpa, until after concentrated solution density is 1.15g/mL, then pour concentrated solution into 3
In the ethanol solution of times volume 95%, after eucommia bark polycose separates out, the method separating polyose that application periosteum filters,
Wherein periosteum molecular cut off 5000D, polysaccharide utilizes the method for vacuum lyophilization to be dried, i.e. obtains finished product
Eucommia bark polycose；
(4) enzymolysis: the filtering residue in step (3) is added distilled water according to the ratio of solid-liquid ratio 1:40,
Regulating pH to 5.2 with sodium acetate, be subsequently adding the compound enzyme of 100IU/g, compound enzyme mainly includes pectase
18000IU/g, xylanase 3500IU/g, cellulase 5500IU/g, 1,4 beta-glucanase >=11000IU/g
Composition, under the conditions of 50 DEG C, after combinative enzyme hydrolysis 36h, utilizes high-pressure cleaning device to rinse lignin residue,
Hydraulic pressure 800bar, obtains the thick glue of the Cortex Eucommiae；
(5) extraction purification: after the thick glue of the Cortex Eucommiae in step (4) is dried process, according to solid-liquid ratio
The ratio of 1:20 and petroleum ether (boiling range: 60～90 DEG C) mixing, under the conditions of 85 DEG C, 1h is extracted in condensation,
Heat filtering goes the removal of impurity, by liquid at-20 DEG C of cold preservation 0.5h, after gutta-percha separates out, reclaims petroleum ether,
Eucommia ulmoides refined glue is i.e. obtained through vacuum drying.
Embodiment 4:
A kind of method extracting separation gutta-percha, comprises the steps:
(1) pre-treatment: by eucommia bark, after roguing processes, according to the prescription of Chinese Pharmacopoeia,
Qualified through inspection, dry eucommia bark machinery suitably to be pulverized, granularity is 12cm, is placed in dry
Dry shady and cool at standby；
(2) steam explosion: the material after pre-treatment is put into steam blasting device and carries out steam explosion,
The pressure of steam explosion is 1.0MPa, and temperature when controlling the steam explosion of steam blasting device is 150 DEG C,
And tie up pressure 3min, after steam explosion, temperature of charge is room temperature；
(3) by filtering residue and the NaOH solution of 1% of step (2), according to the ratio that solid-liquid ratio is 1:15
Example mixes, and extracts 2.5h, after filtration, pump to receiver under the conditions of 65 DEG C, during second extraction, according to
The solid-liquid ratio mixing of 1:8, Extracting temperature is identical with first time with the time, separating filtrate, and filtering residue stores for future use,
After merging twice filtrate, regulate pH5.7 with the hydrochloric acid of 5mol/L, utilize the volume being 300D by molecular weight
Membrance concentration, outlet pressure 0.22Mpa, until after concentrated solution density is 1.11g/mL, then concentrated solution is poured into
In the ethanol solution of 2.2 times of volumes 95%, separate out eucommia bark polycose, apply the method separating polyose that periosteum filters,
Wherein periosteum molecular cut off 2000D, polysaccharide utilizes the method for vacuum lyophilization to be dried, i.e. obtains finished product
Eucommia bark polycose；
(4) enzymolysis: the filtering residue of step (3) is added distilled water according to the ratio of solid-liquid ratio 1:20, uses
Sodium acetate regulation pH to 4.9, is subsequently adding the compound enzyme of 50IU/g, and compound enzyme mainly includes pectase
18000IU/g, xylanase 3500IU/g, cellulase 5500IU/g and 1,4 beta-glucanase >=11000IU/g,
Under the conditions of 51 DEG C, after combinative enzyme hydrolysis 60h, high-pressure cleaning device is utilized to rinse lignin residue, hydraulic pressure
500bar, obtains the thick glue of the Cortex Eucommiae；
(5) after the thick glue of the Cortex Eucommiae that step (4) obtains being dried process, according to the ratio of solid-liquid ratio 1:8
Example and petroleum ether (boiling range: 60～90 DEG C) mixing, under the conditions of 82 DEG C, 3h is extracted in condensation, and heat filtering goes
The removal of impurity, by liquid at-8 DEG C of cold preservation 2.5h, after gutta-percha separates out, reclaims petroleum ether, does through vacuum
Dry i.e. obtain eucommia ulmoides refined glue.
Embodiment 5:
A kind of method extracting separation gutta-percha, comprises the steps:
(1) pre-treatment: by eucommia bark, after roguing processes, according to the prescription of Chinese Pharmacopoeia,
Qualified through inspection, dry eucommia bark machinery suitably to be pulverized, granularity is 15cm, is placed in dry
Dry shady and cool at standby；
(2) steam explosion: the material after pre-treatment is placed in the water of 26 DEG C immersion 16h, then will
Material after immersion is put into steam blasting device and is carried out steam explosion, and the pressure of steam explosion is 1MPa, control
The temperature during steam explosion of steam blasting device processed is 170 DEG C, and ties up pressure 12min, thing after steam explosion
Material temperature degree is room temperature；
(3) by filtering residue and the NaOH solution of 3.2% of step (2), it is 1:14's according to solid-liquid ratio
Ratio mixes, and extracts 1.5h, after filtration, pump to receiver under the conditions of 72 DEG C, during second extraction, according to
The solid-liquid ratio mixing of 1:12, Extracting temperature is identical with first time with the time, separating filtrate, and filtering residue stores for future use,
After merging twice filtrate, with the salt acid for adjusting pH 5.8 of 7mol/L, utilize the volume being 300D by molecular weight
Membrance concentration, outlet pressure 0.28Mpa, until after concentrated solution density is 1.14g/mL, then concentrated solution is poured into
In the ethanol solution of 2.8 times of volumes 95%, separate out eucommia bark polycose, apply the method separating polyose that periosteum filters,
Wherein periosteum molecular cut off 1400D, polysaccharide utilizes the method for vacuum lyophilization to be dried, i.e. obtains finished product
Eucommia bark polycose；
(4) enzymolysis: the filtering residue of step (3) is added distilled water according to the ratio of solid-liquid ratio 1:35, uses
Sodium acetate regulation pH to 5.1, is subsequently adding the compound enzyme of 70IU/g, and compound enzyme mainly includes pectase
18000IU/g, xylanase 3500IU/g, cellulase 5500IU/g and 1,4 beta-glucanase >=11000IU/g,
Under the conditions of 52 DEG C, after combinative enzyme hydrolysis 72h, high-pressure cleaning device is utilized to rinse lignin residue, hydraulic pressure
500bar, obtains the thick glue of the Cortex Eucommiae；
(5) after the thick glue of the Cortex Eucommiae that step (4) obtains being dried process, according to solid-liquid ratio 1:16's
Ratio and petroleum ether (boiling range: 60～90 DEG C) mixing, under the conditions of 84 DEG C, 2h, heat filtering are extracted in condensation
Go the removal of impurity, by liquid at-14 DEG C of cold preservation 1.5h, after gutta-percha separates out, reclaim petroleum ether, Jing Guozhen
Empty drying to obtain eucommia ulmoides refined glue.
Embodiment 6:
A kind of method extracting separation gutta-percha, comprises the steps:
(1) pre-treatment: by eucommia bark, after roguing processes, according to the prescription of Chinese Pharmacopoeia,
Qualified through inspection, dry eucommia bark machinery suitably to be pulverized, granularity is 4cm, is placed in dry
At Yin Liang standby；
(2) steam explosion: the material after pre-treatment is placed in the water of 27 DEG C immersion 20h, then will
Material after immersion is put into steam blasting device and is carried out steam explosion, and the pressure of steam explosion is 1.5MPa,
Temperature when controlling the steam explosion of steam blasting device is 172 DEG C, and ties up pressure 14min, after steam explosion
Temperature of charge is room temperature；
(3) by filtering residue and the NaOH solution of 3.6% of step (2), it is 1:18's according to solid-liquid ratio
Ratio mixes, and extracts 1.2h, after filtration, pump to receiver under the conditions of 78 DEG C, during second extraction, according to
The solid-liquid ratio mixing of 1:15, Extracting temperature is identical with first time with the time, separating filtrate, and filtering residue stores for future use,
After merging twice filtrate, with the salt acid for adjusting pH 5.9 of 7.5mol/L, utilize by molecular weight as 300D's
Wound membrane concentrates, outlet pressure 0.26Mpa, until after concentrated solution density is 1.13g/mL, then concentrated solution is fallen
Entering in the ethanol solution of 2.7 times of volumes 95%, separate out eucommia bark polycose, the method that application periosteum filters separates many
Sugar, wherein periosteum molecular cut off 4500D, polysaccharide utilizes the method for vacuum lyophilization to be dried, i.e. obtains
Finished product eucommia bark polycose；
(4) enzymolysis: the filtering residue of step (3) is added distilled water according to the ratio of solid-liquid ratio 1:25, uses
Sodium acetate regulation pH to 5.1, is subsequently adding the compound enzyme of 80IU/g, and compound enzyme mainly includes pectase
18000IU/g, xylanase 3500IU/g, cellulase 5500IU/g and 1,4 beta-glucanase >=11000IU/g,
Under the conditions of 51 DEG C, after combinative enzyme hydrolysis 80h, high-pressure cleaning device is utilized to rinse lignin residue, hydraulic pressure
500bar, obtains the thick glue of the Cortex Eucommiae；
(5) after the thick glue of the Cortex Eucommiae that step (4) obtains being dried process, according to solid-liquid ratio 1:15's
Ratio and petroleum ether (boiling range: 60～90 DEG C) mixing, under the conditions of 81 DEG C, 2h, heat filtering are extracted in condensation
Go the removal of impurity, by liquid at-15 DEG C of cold preservation 1.5h, after gutta-percha separates out, reclaim petroleum ether, Jing Guozhen
Empty drying to obtain eucommia ulmoides refined glue.
The above, be only presently preferred embodiments of the present invention, not makees the present invention any pro forma
Limit, although the present invention discloses as above with preferred embodiment, but is not limited to the present invention, any
Those skilled in the art, in the range of without departing from technical solution of the present invention, when available the disclosure above
Method and technology contents make a little Equivalent embodiments changed or be modified to equivalent variations, as long as being not
Departing from the content of technical solution of the present invention, it is any that above example is made by the technical spirit of the foundation present invention
Simple modification, equivalent variations and modification, all still fall within the range of technical solution of the present invention.
Claims (6)
1. one kind is extracted the method separating gutta-percha, including pre-treatment, alkali process, enzymolysis and extraction purification step, it is characterized in that: after pre-treatment step, also include steam explosion pre-treatment step, material after pre-treatment is placed in the water of 20～30 DEG C immersion 0～24h, and the material after then soaking is put into steam blasting device and is carried out steam explosion；
The described method extracting separation gutta-percha comprises the following steps:
(1) pre-treatment: by Cortex Eucommiae raw material, roguing processes, and being crushed to particle diameter is 1～15cm, is placed at dry cool place standby；
(2) steam explosion pretreatment: the material after pre-treatment is placed in the water of 20～30 DEG C immersion 0～24h, then the material after soaking is put into steam blasting device and is carried out steam explosion, the pressure of steam explosion is 0.5～1.8MPa, temperature when controlling the steam explosion of steam blasting device is 140～180 DEG C, dimension pressure 1～15min, after steam explosion, temperature of charge is room temperature；
(3) alkali processes: use NaOH solution to extract twice the filtering residue of step (2), merge twice filtrate, salt acid for adjusting pH is to 5.5～6.0, concentrated solution is poured in ethanol solution after concentrating by wound membrane, separate out eucommia bark polycose, filter, separate eucommia bark polycose, it is dried, obtains finished product eucommia bark polycose；
(4) enzymolysis: the filtering residue in step (3) is added distilled water, with vinegar acid for adjusting pH to 4.8～5.2, is subsequently adding combinative enzyme hydrolysis, rinses lignin residue, obtain the thick glue of the Cortex Eucommiae；
(5) extraction purification: mix with petroleum ether after the Cortex Eucommiae thick glue dried that step (4) is obtained, condensation extraction, heat filtering remove impurity, filtrate cold preservation, separate out gutta-percha, reclaim petroleum ether, vacuum drying obtains eucommia ulmoides refined glue.
nullA kind of method extracting separation gutta-percha the most according to claim 1，It is characterized in that: described step (3) is particularly as follows: by the filtering residue of step (2) and 0.5～the NaOH solution of 4%，According to the ratio mixing that solid-liquid ratio is 1:5～1:20，1～3h is extracted under the conditions of 60～80 DEG C，After filtration，Pump is to receiver，During second extraction，Mix according to the solid-liquid ratio of 1:5～1:15，Extracting temperature is identical with first time with the time，Separating filtrate，Filtering residue stores for future use，After merging twice filtrate，Salt acid for adjusting pH 5.5～6.0 with 4～8mol/L，The wound membrane being 300D by molecular weight is utilized to concentrate，Outlet pressure 0.2～0.3Mpa，Until after concentrated solution density is 1.10～1.15g/mL，Again concentrated solution is poured in the ethanol solution of 2～3 times of volumes 95%，Separate out eucommia bark polycose，The method separating polyose that application periosteum filters，Wherein periosteum molecular cut off 1000～5000D，Polysaccharide utilizes the method for vacuum lyophilization to be dried，I.e. obtain finished product eucommia bark polycose.
A kind of method extracting separation gutta-percha the most according to claim 1 and 2, it is characterized in that: described eucommia bark polycose mainly includes rhamnosan >=1.66%, arabinan >=6.72%, mannan >=4.11%, glucosan >=6.42%, xylan >=4.75%, glucuronic acid >=1.65%.
A kind of method extracting separation gutta-percha the most according to claim 1, it is characterized in that: described step (4) is particularly as follows: add distilled water by the filtering residue of step (3) according to the ratio of solid-liquid ratio 1:10～1:40, pH to 4.8～5.2 is regulated with sodium acetate, it is subsequently adding the compound enzyme of 30～100IU/g, under the conditions of 48～52 DEG C, after combinative enzyme hydrolysis 36～84h, high-pressure cleaning device is utilized to rinse lignin residue, hydraulic pressure 100bar～800bar, obtains the thick glue of the Cortex Eucommiae.
A kind of method extracting separation gutta-percha the most according to claim 4, it is characterised in that: described compound enzyme mainly includes pectase 18000IU/g, xylanase 3500IU/g, cellulase 5500IU/g and 1,4 beta-glucanase >=11000IU/g.
A kind of method extracting separation gutta-percha the most according to claim 1, it is characterized in that: described step (5) is particularly as follows: after the thick glue of the Cortex Eucommiae that step (4) obtained is dried process, ratio and petroleum ether mixing, the boiling range of petroleum ether: 60～90 DEG C according to solid-liquid ratio 1:5～1:20；Under the conditions of 80～85 DEG C, condensation extracts 1～4h, and heat filtering goes the removal of impurity, by liquid-4～-20 DEG C of cold preservations 0.5～3h, after gutta-percha separates out, reclaims petroleum ether, i.e. obtains eucommia ulmoides refined glue through vacuum drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410500227.2A CN104231281B (en) | 2014-09-26 | 2014-09-26 | A kind of method extracting separation gutta-percha |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410500227.2A CN104231281B (en) | 2014-09-26 | 2014-09-26 | A kind of method extracting separation gutta-percha |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104231281A CN104231281A (en) | 2014-12-24 |
| CN104231281B true CN104231281B (en) | 2016-11-16 |
Family
ID=52220254
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410500227.2A Active CN104231281B (en) | 2014-09-26 | 2014-09-26 | A kind of method extracting separation gutta-percha |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104231281B (en) |
Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104479143B (en) * | 2014-11-26 | 2017-03-29 | 国家***泡桐研究开发中心 | A kind of method of supersonic speed steam explosion separation and Extraction gutta percha |
| CN105111465A (en) * | 2015-09-23 | 2015-12-02 | 成都艾比科生物科技有限公司 | Method for extracting filament gutta-percha from eucommia ulmoides by adopting solvent method |
| CN105524287B (en) * | 2016-02-01 | 2017-12-19 | 吉首大学 | Fermentation leaching combines the method that gutta-percha is extracted from bark of eucommia shell |
| CN106107341A (en) * | 2016-06-24 | 2016-11-16 | 广西灵山县宇峰保健食品有限公司 | A kind of Herba mesonae chinensis beverage and preparation method thereof |
| CN106071557A (en) * | 2016-06-24 | 2016-11-09 | 广西灵山县宇峰保健食品有限公司 | Herba mesonae chinensis beverage and preparation method thereof |
| CN108047356B (en) * | 2018-01-29 | 2020-06-16 | 山东贝隆杜仲生物工程有限公司 | Method for refining eucommia ulmoides crude glue solution |
| CN107987186B (en) * | 2018-01-29 | 2020-07-03 | 山东贝隆杜仲生物工程有限公司 | Purification process of eucommia ulmoides crude gum |
| CN108392669A (en) * | 2018-03-01 | 2018-08-14 | 澳门大学 | A kind of bioactive polysaccharide dressing and its preparation method and application for wound repair |
| CN110302234A (en) * | 2019-08-08 | 2019-10-08 | 国家林业和草原局泡桐研究开发中心 | The method of comprehensive utilization of Cortex Eucommiae and the solution containing eucommia ulmoides extracts for using this method to obtain or the solid containing gutta-percha |
| CN111333070B (en) * | 2020-03-10 | 2022-09-16 | 天津科技大学 | Method for utilizing whole components of sunflower disc raw material |
| CN113801341A (en) * | 2020-06-15 | 2021-12-17 | 广州中国科学院先进技术研究所 | Method for extracting, concentrating and recovering organic solvent from gutta-percha |
| CN115068975B (en) * | 2022-06-09 | 2024-05-17 | 新疆汇峰农业科技有限公司 | Cistanche stock solution production method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351700A (en) * | 2011-08-15 | 2012-02-15 | 中国科学院过程工程研究所 | Method for separating and purifying chlorogenic acid from eucommia ulmoides leaves |
| CN102977380A (en) * | 2012-12-21 | 2013-03-20 | 吉首大学 | Method for extracting high-purity gutta-percha from cortex eucommiae key fruit |
-
2014
- 2014-09-26 CN CN201410500227.2A patent/CN104231281B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351700A (en) * | 2011-08-15 | 2012-02-15 | 中国科学院过程工程研究所 | Method for separating and purifying chlorogenic acid from eucommia ulmoides leaves |
| CN102977380A (en) * | 2012-12-21 | 2013-03-20 | 吉首大学 | Method for extracting high-purity gutta-percha from cortex eucommiae key fruit |
Non-Patent Citations (1)
| Title |
|---|
| 何国菊.杜仲籽中油和杜仲胶的提取工艺研究.《贵阳学院学报(自然科学版) (季刊)》.2011,第6卷(第1期),第14-18页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104231281A (en) | 2014-12-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104231281B (en) | A kind of method extracting separation gutta-percha | |
| CN104292352B (en) | A kind of Cortex Eucommiae fine powder, eucommia bark polycose and gutta-percha coproduction extraction separation method | |
| CN105032282A (en) | Preparation method for high-purity gleditsia sinensis natural surfactant | |
| CN107385001A (en) | Process for extracting sea cucumber oligopeptide and sea cucumber polysaccharide from sea cucumber deep-processing byproducts | |
| CN102432664A (en) | Method for extracting theasaponin from tea seed pulp | |
| CN103804503A (en) | Method of extracting polysaccharide of enteromorpha by enzymolysis in steps | |
| CN103304678B (en) | A kind of method utilizing multiplex-enzyme extraction Alfalfa Polysaccharide | |
| CN103641924A (en) | Method for extraction of Auricularia auricula polysaccharide from Auricularia auricula | |
| CN104026706B (en) | A kind of preparation method of red bamboo liquid | |
| CN103965152A (en) | Extraction and preparation method for licorice effective ingredients | |
| CN107411081A (en) | A kind of Methods of Extraction of Tea-polyphenols | |
| CN104311698A (en) | Kelp deep processing method | |
| CN101830995B (en) | Method for extracting polysaccharide by adopting decompressing inner ebullition | |
| CN105272887A (en) | Method for extracting taurine and polysaccharides from abalone's viscera simultaneously | |
| CN104231282B (en) | A kind of extraction from Eucommia separates eucommia ulmoides seed oil and the method for gutta-percha | |
| CN104495754A (en) | Extraction method of algae iodate and composite algae iodate salt additive | |
| CN105859916A (en) | Preparing method for NO.9 south jerusalem artichoke powder | |
| CN103626887B (en) | A kind of method of preparing sugarcane tip polysaccharide with the sugarcane tip | |
| CN105237339A (en) | Method for extracting octacosanol by using sugar refinery mixing juice floating residue as raw material | |
| CN102181076A (en) | Method for cleanly preparing starch containing abundant flavones and comprehensively utilizing radix puerariae resource | |
| CN109077185A (en) | The preparation method of natural saccharicter-penin | |
| CN104497122A (en) | Method for extracting gastric mucin from porcine gastric mucosa | |
| CN104151377A (en) | Technology and method for extraction of teasaponin from Camellia oleifera Abel seed meal | |
| CN104013065B (en) | A kind of preparation method of red bamboo liquid | |
| CN103860637A (en) | Preparing method of total alkali liquor of sophora alopecuroide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |