CN109206307A - The extraction and preparation process of juglone in a kind of green peel of walnut - Google Patents
The extraction and preparation process of juglone in a kind of green peel of walnut Download PDFInfo
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- CN109206307A CN109206307A CN201810885750.XA CN201810885750A CN109206307A CN 109206307 A CN109206307 A CN 109206307A CN 201810885750 A CN201810885750 A CN 201810885750A CN 109206307 A CN109206307 A CN 109206307A
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- walnut
- juglone
- green peel
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C46/00—Preparation of quinones
- C07C46/10—Separation; Purification; Stabilisation; Use of additives
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Abstract
The present invention relates to the extractions and preparation process of juglone in a kind of green peel of walnut, it is the following steps are included: step A, feedstock processing, step B, complex enzyme hydrolysis, step C, step D, ultrasonic wave extraction is concentrated by evaporation, step E, be freeze-dried, step F, step G, low-temperature grinding is packed；The method that disclosure sets forth a kind of to extract and prepare juglone from green peel of walnut, it solves the problems, such as to turn waste into wealth green peel of walnut, up to 96% or more, juglone yield has highly application value the juglone extract relative amount that this method is extracted up to 0.0903% or more；The present invention has the advantages that stablize feasible, high suitable for large-scale production, application value.
Description
Technical field
The invention belongs to the extractions and preparation of juglone in juglone extractive technique field more particularly to a kind of green peel of walnut
Technique.
Background technique
Walnut is the higher a kind of crop of economic value in Juglans plants, the end of the year 2015 with a long history in Chinese cultivated
Chinese walnut cultivated area has reached 52,750,000 mu, and about 700,000 tons of yield, and yield is also increasing year by year；Green peel of walnut and core
The ratio of peach nut is about 2.5:1, is the by-product of walnut crop, is seldom utilized at present；Modern research shows that green peel of walnut
In juglone rich in；Juglone (English name: 5-Hydroxy-1,4-naphthoquinone), ((hydroxyl -1 5-,
4- naphthoquinones) it is that a kind of naphthoquinones class active material separated is extracted from juglans mandshurica；1985, for the first time from the green peel of walnut
Separating-purifying goes out juglone, and identifies structure；English walnut quinone content is higher in fresh green peel of walnut, reaches 0.42%, with storage
The extension of time, English walnut quinone content gradually decrease；Modern medicine study shows that juglone has apparent antibacterial and antitumaous effect,
Quinones substance in green peel of walnut has apparent inhibiting effect to a variety of internal transplanted tumors, and the effect of Cytotoxicity in vitro cell is more
By force, and toxicity is lower；Juglone has very wide prospect as a kind of exploitation of natural nuisance-free product；But adding
Walnut fruit regards a treasured as by everybody when work walnut, but has ignored green peel of walnut, the green peel of walnut after processing arbitrarily abandons, very not
Know containing numerous chemical toxicants in Cortex walnut, if dealt with improperly, can greatly pollute the environment on periphery；Therefore it provides a kind of
Stablize the extraction and preparation process right and wrong of juglone in green peel of walnut feasible, high suitable for large-scale production, application value
Often it is necessary to.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, and provide it is a kind of stablize it is feasible, be suitable for large-scale production,
The extraction and preparation process of juglone in the high green peel of walnut of application value.
The technical scheme is that: the extraction and preparation process of juglone in a kind of green peel of walnut, it the following steps are included:
Step A, feedstock processing: selecting fresh green peel of walnut, with thermostatic drying chamber 40 DEG C at a temperature of be dried, when dry
Between be 4h, then the later green peel of walnut of drying is ground into 40 mesh powders with medicinal herb grinder, is sieved, adds pure water retting,
And generate slurry；
Step B, complex enzyme hydrolysis: adding cellulase and pectase in the impregnated slurry of previous step, is 25 DEG C in temperature
Under the conditions of, adjustment pH value is 4.5, with blender with the speed stirring hydrolysis 120min of 10-12r/min；
Step C, ultrasonic wave extraction: the slurry after previous step is digested is mixed according to the weight proportion of 1:9 with chloroform, mixed
Mixture is ultrasonically treated 30min in ultrasonic extraction equipment, generates extracting solution；
Step D, it is concentrated by evaporation: the extracting solution that previous step generates being concentrated by evaporation under low temperature, vacuum condition, obtains concentrate；
Step E, it is freeze-dried: the concentrate that previous step generates is freeze-dried with freeze drier, obtain honeycomb recklessly
Peach quinone solid；
Step F, low-temperature grinding: the juglone solid that previous step is generated, in the pulverizer equipped with ice water cooling system, in 5-
Under the conditions of 10 DEG C of temperature, crush as 60 mesh powders, sieving；
Step G, pack: the juglone powder after previous step is sieved is dispensed into clad aluminum foil bag, and nitrogen charging sealing prints day
Phase is stored at room temperature after vanning.
The specific steps for [adding pure water retting] in the step A are as follows: by green peel of walnut powder and pure water according to 1:
1.2 weight proportion is mixed, and is stirred evenly, and 3h is then impregnated；The temperature of the pure water is 15-20 DEG C, conductivity
Less than 10us/cm.
The concentration of cellulase in the step B is 450ppm, and the concentration of the pectase is 350ppm.
The power of ultrasonic extraction equipment in the step C is 40KHz.
[low temperature, vacuum condition] in the step D is 30-35 DEG C, vacuum degree 75-85KPa, the step D
Concentrate be concentrate that soluble solid content is 30-35%.
The invention has the following advantages that the present invention uses cellulase and pectase, fiber in walnut black cloth can be digested
Element and colloid dissolve conducive to the release of juglone, using ultrasonic extraction equipment, improve recovery rate, reduce production cost,
Using being concentrated by evaporation and being freeze-dried, the pure natural character of juglone is maintained to the maximum extent, meets the green of modern consumption
Concept；The present invention extracts and prepares juglone using fresh walnut black cloth, is suitble to large-scale production and promotes, and has preferable warp
Ji benefit, and avoid pollution of the walnut black cloth for environment；The present invention have stablize it is feasible, suitable for being mass produced, pushing away
The high advantage of wide application value.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated.
Embodiment 1
The extraction and preparation process of juglone in a kind of green peel of walnut, it the following steps are included:
Step A, feedstock processing: selecting fresh green peel of walnut, with thermostatic drying chamber 40 DEG C at a temperature of be dried, when dry
Between be 4h, then the later green peel of walnut of drying is ground into 40 mesh powders with medicinal herb grinder, is sieved, adds pure water retting,
And generate slurry；
Step B, complex enzyme hydrolysis: adding cellulase and pectase in the impregnated slurry of previous step, is 25 DEG C in temperature
Under the conditions of, adjustment pH value is 4.5, with blender with the speed stirring hydrolysis 120min of 10-12r/min；
Step C, ultrasonic wave extraction: the slurry after previous step is digested is mixed according to the weight proportion of 1:9 with chloroform, mixed
Mixture is ultrasonically treated 30min in ultrasonic extraction equipment, generates extracting solution；
Step D, it is concentrated by evaporation: the extracting solution that previous step generates being concentrated by evaporation under low temperature, vacuum condition, obtains concentrate；
Step E, it is freeze-dried: the concentrate that previous step generates is freeze-dried with freeze drier, obtain honeycomb recklessly
Peach quinone solid；
Step F, low-temperature grinding: the juglone solid that previous step is generated, in the pulverizer equipped with ice water cooling system, in 5-
It under the conditions of 6 DEG C of temperature, crushes as 60 mesh powders, sieving, the aperture of sieve is 60 mesh；
Step G, pack: the juglone powder after previous step is sieved is dispensed into clad aluminum foil bag, and nitrogen charging sealing prints day
Phase is stored at room temperature after vanning.
The specific steps for [adding pure water retting] in the step A are as follows: by green peel of walnut powder and pure water according to 1:
1.2 weight proportion is mixed, and is stirred evenly, and 3h is then impregnated；The temperature of the pure water is 15-16 DEG C, conductivity
Less than 10us/cm.
The concentration of cellulase in the step B is 450ppm, and the concentration of the pectase is 350ppm.
The power of ultrasonic extraction equipment in the step C is 40KHz.
[low temperature, vacuum condition] in the step D is 30-32 DEG C, vacuum degree 75-78KPa, the step D
Concentrate be concentrate that soluble solid content is 30-35%.
The present invention uses cellulase and pectase, can digest cellulose and colloid in walnut black cloth, is conducive to juglone
Release dissolution, using ultrasonic extraction equipment, improve recovery rate, reduce production cost, using be concentrated by evaporation and freezing
It is dry, the pure natural shape of juglone is maintained to the maximum extent, meets the green concept of modern consumption；The present invention utilizes fresh
Walnut black cloth extracts and prepares juglone, is suitble to large-scale production and promotes, has preferable economic benefit, and avoid core
Pollution of the peach black cloth for environment；The method that disclosure sets forth a kind of to extract and prepare juglone from green peel of walnut solves
The problem of green peel of walnut is turned waste into wealth, up to 96% or more, juglone obtains the juglone extract relative amount that this method is extracted
Rate has highly application value up to 0.00803% or more；The present invention have stablize it is feasible, be suitable for large-scale production,
The high advantage of application value.
Embodiment 2
The extraction and preparation process of juglone in a kind of green peel of walnut, it the following steps are included:
Step A, feedstock processing: selecting fresh green peel of walnut, with thermostatic drying chamber 40 DEG C at a temperature of be dried, when dry
Between be 4h, then the later green peel of walnut of drying is ground into 40 mesh powders with medicinal herb grinder, is sieved, adds pure water retting,
And generate slurry；
Step B, complex enzyme hydrolysis: adding cellulase and pectase in the impregnated slurry of previous step, is 25 DEG C in temperature
Under the conditions of, adjustment pH value is 4.5, with blender with the speed stirring hydrolysis 120min of 10-12r/min；
Step C, ultrasonic wave extraction: the slurry after previous step is digested is mixed according to the weight proportion of 1:9 with chloroform, mixed
Mixture is ultrasonically treated 30min in ultrasonic extraction equipment, generates extracting solution；
Step D, it is concentrated by evaporation: the extracting solution that previous step generates being concentrated by evaporation under low temperature, vacuum condition, obtains concentrate；
Step E, it is freeze-dried: the concentrate that previous step generates is freeze-dried with freeze drier, obtain honeycomb recklessly
Peach quinone solid；
Step F, low-temperature grinding: the juglone solid that previous step is generated, in the pulverizer equipped with ice water cooling system, in 6-
It under the conditions of 8 DEG C of temperature, crushes as 60 mesh powders, sieving, the aperture of sieve is 60 mesh；
Step G, pack: the juglone powder after previous step is sieved is dispensed into clad aluminum foil bag, and nitrogen charging sealing prints day
Phase is stored at room temperature after vanning.
The specific steps for [adding pure water retting] in the step A are as follows: by green peel of walnut powder and pure water according to 1:
1.2 weight proportion is mixed, and is stirred evenly, and 3h is then impregnated；The temperature of the pure water is 16-18 DEG C, conductivity
Less than 10us/cm.
The concentration of cellulase in the step B is 450ppm, and the concentration of the pectase is 350ppm.
The power of ultrasonic extraction equipment in the step C is 40KHz.
[low temperature, vacuum condition] in the step D is 32-33 DEG C, vacuum degree 78-82KPa, the step D
Concentrate be concentrate that soluble solid content is 30-35%.
The present invention uses cellulase and pectase, can digest cellulose and colloid in walnut black cloth, is conducive to juglone
Release dissolution, using ultrasonic extraction equipment, improve recovery rate, reduce production cost, using be concentrated by evaporation and freezing
It is dry, the pure natural shape of juglone is maintained to the maximum extent, meets the green concept of modern consumption；The present invention utilizes fresh
Walnut black cloth extracts and prepares juglone, is suitble to large-scale production and promotes, has preferable economic benefit, and avoid core
Pollution of the peach black cloth for environment；The method that disclosure sets forth a kind of to extract and prepare juglone from green peel of walnut solves
The problem of green peel of walnut is turned waste into wealth, juglone extract relative amount that this method is extracted is up to 96% or more, juglone
Yield has highly application value up to 0.00803% or more；The present invention have stablize it is feasible, be suitable for it is extensive raw
It produces, the advantage that application value is high.
Embodiment 3
The extraction and preparation process of juglone in a kind of green peel of walnut, it the following steps are included:
Step A, feedstock processing: selecting fresh green peel of walnut, with thermostatic drying chamber 40 DEG C at a temperature of be dried, when dry
Between be 4h, then the later green peel of walnut of drying is ground into 40 mesh powders with medicinal herb grinder, is sieved, adds pure water retting,
And generate slurry；
Step B, complex enzyme hydrolysis: adding cellulase and pectase in the impregnated slurry of previous step, is 25 DEG C in temperature
Under the conditions of, adjustment pH value is 4.5, with blender with the speed stirring hydrolysis 120min of 10-12r/min；
Step C, ultrasonic wave extraction: the slurry after previous step is digested is mixed according to the weight proportion of 1:9 with chloroform, mixed
Mixture is ultrasonically treated 30min in ultrasonic extraction equipment, generates extracting solution；
Step D, it is concentrated by evaporation: the extracting solution that previous step generates being concentrated by evaporation under low temperature, vacuum condition, obtains concentrate；
Step E, it is freeze-dried: the concentrate that previous step generates is freeze-dried with freeze drier, obtain honeycomb recklessly
Peach quinone solid；
Step F, low-temperature grinding: the juglone solid that previous step is generated, in the pulverizer equipped with ice water cooling system, in 8-
It under the conditions of 10 DEG C of temperature, crushes as 60 mesh powders, sieving, the aperture of sieve is 60 mesh；
Step G, pack: the juglone powder after previous step is sieved is dispensed into clad aluminum foil bag, and nitrogen charging sealing prints day
Phase is stored at room temperature after vanning.
The specific steps for [adding pure water retting] in the step A are as follows: by green peel of walnut powder and pure water according to 1:
1.2 weight proportion is mixed, and is stirred evenly, and 3h is then impregnated；The temperature of the pure water is 18-20 DEG C, conductivity
Less than 10us/cm.
The concentration of cellulase in the step B is 450ppm, and the concentration of the pectase is 350ppm.
The power of ultrasonic extraction equipment in the step C is 40KHz.
[low temperature, vacuum condition] in the step D is 33-35 DEG C, vacuum degree 82-85KPa, the step D
Concentrate be concentrate that soluble solid content is 30-35%.
The present invention uses cellulase and pectase, can digest cellulose and colloid in walnut black cloth, is conducive to juglone
Release dissolution, using ultrasonic extraction equipment, improve recovery rate, reduce production cost, using be concentrated by evaporation and freezing
It is dry, the pure natural shape of juglone is maintained to the maximum extent, meets the green concept of modern consumption；The present invention utilizes fresh
Walnut black cloth extracts and prepares juglone, is suitble to large-scale production and promotes, has preferable economic benefit, and avoid core
Pollution of the peach black cloth for environment；The method that disclosure sets forth a kind of to extract and prepare juglone from green peel of walnut solves
The problem of green peel of walnut is turned waste into wealth, up to 96% or more, juglone obtains the juglone extract relative amount that this method is extracted
Rate has highly application value up to 0.00803% or more；The present invention have stablize it is feasible, be suitable for large-scale production,
The high advantage of application value.
Performance in order to further illustrate the present invention, the following provide specific experiment samples:
| Specific implementation | Green peel of walnut weight (unit: Kg) | Juglone weight (unit: g) | Yield |
| Embodiment 1 | 1000 | 80.39 | 0.008039% |
| Embodiment 2 | 1000 | 80.41 | 0.008041% |
| Embodiment 3 | 1000 | 80.38 | 0.008038% |
Claims (5)
1. the extraction and preparation process of juglone in a kind of green peel of walnut, it is characterised in that: it the following steps are included:
Step A, feedstock processing: selecting fresh green peel of walnut, with thermostatic drying chamber 40 DEG C at a temperature of be dried, when dry
Between be 4h, then the later green peel of walnut of drying is ground into 40 mesh powders with medicinal herb grinder, is sieved, adds pure water retting,
And generate slurry；
Step B, complex enzyme hydrolysis: adding cellulase and pectase in the impregnated slurry of previous step, is 25 DEG C in temperature
Under the conditions of, adjustment pH value is 4.5, with blender with the speed stirring hydrolysis 120min of 10-12r/min；
Step C, ultrasonic wave extraction: the slurry after previous step is digested is mixed according to the weight proportion of 1:9 with chloroform, mixed
Mixture is ultrasonically treated 30min in ultrasonic extraction equipment, generates extracting solution；
Step D, it is concentrated by evaporation: the extracting solution that previous step generates being concentrated by evaporation under low temperature, vacuum condition, obtains concentrate；
Step E, it is freeze-dried: the concentrate that previous step generates is freeze-dried with freeze drier, obtain honeycomb recklessly
Peach quinone solid；
Step F, low-temperature grinding: the juglone solid that previous step is generated, in the pulverizer equipped with ice water cooling system, in 5-
Under the conditions of 10 DEG C of temperature, crush as 60 mesh powders, sieving；
Step G, pack: the juglone powder after previous step is sieved is dispensed into clad aluminum foil bag, and nitrogen charging sealing prints day
Phase is stored at room temperature after vanning.
2. the extraction and preparation process of juglone in a kind of green peel of walnut as described in claim 1, it is characterised in that: described
The specific steps for [adding pure water retting] in step A are as follows: by green peel of walnut powder and pure water according to 1:1.2 weight proportion into
Row mixing, stirs evenly, then impregnates 3h；The temperature of the pure water is 15-20 DEG C, conductivity is less than 10us/cm.
3. the extraction and preparation process of juglone in a kind of green peel of walnut as described in claim 1, it is characterised in that: described
The concentration of cellulase in step B is 450ppm, and the concentration of the pectase is 350ppm.
4. the extraction and preparation process of juglone in a kind of green peel of walnut as described in claim 1, it is characterised in that: described
The power of ultrasonic extraction equipment in step C is 40KHz.
5. the extraction and preparation process of juglone in a kind of green peel of walnut as described in claim 1, it is characterised in that: described
[low temperature, vacuum condition] in step D is 30-35 DEG C, the concentrate of vacuum degree 75-85KPa, the step D are solvable
Property solid content be 30-35% concentrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810885750.XA CN109206307A (en) | 2018-08-06 | 2018-08-06 | The extraction and preparation process of juglone in a kind of green peel of walnut |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810885750.XA CN109206307A (en) | 2018-08-06 | 2018-08-06 | The extraction and preparation process of juglone in a kind of green peel of walnut |
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| CN109206307A true CN109206307A (en) | 2019-01-15 |
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| CN201810885750.XA Pending CN109206307A (en) | 2018-08-06 | 2018-08-06 | The extraction and preparation process of juglone in a kind of green peel of walnut |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110229054A (en) * | 2019-07-19 | 2019-09-13 | 商洛学院 | A kind of preparation method of green peel of walnut juglone extract and its application in the prevention and treatment of Chinese medicine root rot |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103319321A (en) * | 2013-06-09 | 2013-09-25 | 吕梁学院 | Extraction method of juglone and derivative in walnut green tangerine peel |
| CN106805180A (en) * | 2017-01-13 | 2017-06-09 | 江南大学 | A kind of method that polyphenol substance is extracted in desmoenzyme and the ultrasonically treated endotesta walnut kernel by band |
-
2018
- 2018-08-06 CN CN201810885750.XA patent/CN109206307A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103319321A (en) * | 2013-06-09 | 2013-09-25 | 吕梁学院 | Extraction method of juglone and derivative in walnut green tangerine peel |
| CN106805180A (en) * | 2017-01-13 | 2017-06-09 | 江南大学 | A kind of method that polyphenol substance is extracted in desmoenzyme and the ultrasonically treated endotesta walnut kernel by band |
Non-Patent Citations (1)
| Title |
|---|
| 冉翠香等: "酶法辅助超声波微波仪从胡桃青皮中提取胡桃醌的工艺研究", 《氨基酸和生物资源》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110229054A (en) * | 2019-07-19 | 2019-09-13 | 商洛学院 | A kind of preparation method of green peel of walnut juglone extract and its application in the prevention and treatment of Chinese medicine root rot |
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