CN105708894A - Method for preparing walnut green husk polyphenol from fresh walnut green husks - Google Patents
Method for preparing walnut green husk polyphenol from fresh walnut green husks Download PDFInfo
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- CN105708894A CN105708894A CN201610107933.XA CN201610107933A CN105708894A CN 105708894 A CN105708894 A CN 105708894A CN 201610107933 A CN201610107933 A CN 201610107933A CN 105708894 A CN105708894 A CN 105708894A
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- polyphenol
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- exocarpium juglandis
- juglandis immaturus
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/52—Juglandaceae (Walnut family)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/31—Extraction of the material involving untreated material, e.g. fruit juice or sap obtained from fresh plants
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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Abstract
The invention relates to a method for preparing walnut green husk polyphenol from fresh walnut green husks and belongs to the technical field of walnut green husk polyphenol preparation. The technological process of the method includes the steps that fresh walnut green husks are juiced, centrifuged and subjected to solid and liquid separation, after the pH value of liquid is adjusted to be 3-4, the liquid is added into a chromatographic column in which AB-8 type resin is contained with the polyphenol concentration of the sample adding liquid being 2-3 mg/mL, pH of the sample adding liquid being 3-4, the volume of added samples being 1.6 BV and the flowing speed of the added samples being 2 BV/h, washing is performed with water, after liquid flowing out of the lower portion of the chromatographic column is colorless, elution is performed with a 65-75% ethyl alcohol, the flowing speed of elution is 1-2 BV/h, and the volume of elution is 2.10 BV. 65-75% of ethyl alcohol eluant is collected, vacuum concentration is performed, and the walnut green husk polyphenol with the content being 53% is obtained through vacuum drying. Compared with a traditional method, the steps of drying the walnut green husks and extracting the walnut green husks with an organic solvent are reduced, the contact time between the green husks and air is shortened, oxidization of the walnut green husk polyphenol is reduced, polyphenol substances are effectively protected, and the consumption of heat and the organic solvent is remarkably reduced.
Description
Technical field
The present invention relates to a kind of method preparing Exocarpium Juglandis Immaturus polyphenol from fresh Exocarpium Juglandis Immaturus, belong to Exocarpium Juglandis Immaturus polyphenol
Preparing technical field.
Background technology
Exocarpium Juglandis Immaturus (walnut green husk) has another name called the Semen Juglandis Green Dragon, is the green outer fruit that the outside thick layer of Semen Juglandis is thick
Skin.Exocarpium Juglandis Immaturus acrid in the mouth is bitter, and property is puckery puts down, be slightly cold, and has heat-clearing and toxic substances removing, dispel the wind treatment tinea, pain relieving dysentery-stopping efficacy, modern pharmacological research
Show that Exocarpium Juglandis Immaturus has antitumor, analgesia, anti-inflammation isoreactivity.Exocarpium Juglandis Immaturus is rich in polyphenol, and polyphenol has antioxidation, resists
Radiation, antiviral, blood fat reducing, antibacterial, slow down aging, raising body immunity, suppression hyperlipemia T-CHOL (TC), glycerol
Three esters (TG) raise, suppress liver lipid peroxidation, improve superoxide dismutase (SOD) vigor, minimizing free radical generation, prevention
Act on treatment hyperlipemia, suppression cardiovascular disease etc..
The Exocarpium Juglandis Immaturus polyphenol method for extraction and purification now reported has:
1, the Exocarpium Juglandis Immaturus powder with drying and crushing carries for raw material through ethanol water, organic solvent extracts walnut green husk total tannin
Method (ZL2009100700385)；
2, extracting with the mix supersonic wave wall breaking that adds water after pulverizing with Exocarpium Juglandis Immaturus, solid-liquid separation, molecule ultrafilter membrane classification divides
From purification, then NF membrane concentrates, and decompression outer circulation concentrates, microwave drying, it is thus achieved that the method for Exocarpium Juglandis Immaturus tannic acid
(ZL2011101155114)；
3, a kind of Exocarpium Juglandis Immaturus dried and crushed, with pectase and cellulase aqueous solution enzymolysis, enzymolysis solution gelatin precipitation, sinks
Shallow lake thing ethyl acetate extraction, extract alumina column chromatography separate the method (CN2013102461953) obtaining walnut tannin；
4, a kind of method (CN2015106713562) of Subcritical water chromotagraphy Exocarpium Juglandis Immaturus pink colour element polyphenol；
5, a kind of method (CN2014103330145) of ultrasonic water extraction Exocarpium Juglandis Immaturus powder polyphenol；
6, Zhu Xia, Liu Yucong, Wu Zhenlin, Guo Lijuan, Luo You, Li Huanrong. it is blue or green that response phase method Optimization for Ultrasonic Wave extracts Semen Juglandis
The technical study [J] of skin polyphenol. food section, 2014,39 (11): 207～211；
7, the macroporous adsorbent resin isolated and purified Exocarpium Juglandis Immaturus total polyphenols method of the Exocarpium Juglandis Immaturus polyphenol extractum of ethanol extraction
[Li Qiong, Chen Kai, Chen Yanqin, Li Huanrong. macroporous adsorbent resin isolated and purified Exocarpium Juglandis Immaturus total polyphenols [J]. food and machinery,
2015,31 (1): 175～180].
Said method all uses the Exocarpium Juglandis Immaturus powder of drying and crushing, carries with water or ethanol or methanol-water extract, enter
Row is isolated and purified；There is fresh Exocarpium Juglandis Immaturus need to first be dried, need consumption of calorie, natural drying time length and Semen Juglandis results season
Solar term are waited pole and are unfavorable for natural drying, and extraction purification needs a large amount of organic solvents, dry and Extracting temperature is higher, effective ingredient is easy
Destroyed problem.
China's Semen Juglandis cultivated area and yield all rank first in the world, and rank first in the whole country again in Yunnan, and its cultivated area exceedes
24000000 mu, Semen Juglandis is gathered period, and substantial amounts of Exocarpium Juglandis Immaturus is discarded in field, the edge of a field or limes marginis, not only cause environmental pollution and
The wasting of resources, also can produce Allelopathy, disturb the growth and breeding of other plant, and the exploitation strengthening Exocarpium Juglandis Immaturus resource are ground
Studying carefully, the sound development to Walnut Industry is significant.
Summary of the invention
It is an object of the invention to overcome the existing deficiency prepared from Exocarpium Juglandis Immaturus in the many phenol methods of Exocarpium Juglandis Immaturus, and carry
For a kind of method preparing Pericarpium Citri Reticulatae Viride polyphenol from fresh Exocarpium Juglandis Immaturus.
A kind of method preparing Exocarpium Juglandis Immaturus polyphenol from fresh Exocarpium Juglandis Immaturus of the present invention, it is not necessary to blue or green to fresh Semen Juglandis
Skin is dried, pulverizes and extracts, and specifically includes following steps:
A) strip fresh Exocarpium Juglandis Immaturus, squeeze the juice with juice extractor；
B) by aforementioned juice in 3000～4500 revs/min, centrifugal 10～20 minutes, supernatant liquid and following is separated afterwards
Residue；
C) pH value of supernatant liquid step b obtained is adjusted to 3～4, mixing；
D) solution step c obtained with sample solution polyphenol concentration 2-3mg/mL, sample solution pH3～4, loading volume is
1.6BV, loading flow velocity is that 2BV/h joins in its chromatographic column built with 1000-2000 gram of AB-8 type resin；
E) chromatographic column in step d adds water, be washed with water to the liquid colorless flowed out below chromatographic column；
F) with the chromatographic column in ethanol elution step e that percentage by volume is 65%～75%, elution flow rate 1～2BV/h,
Elution volume 2.10BV；
G) eluent flowed out below chromatographic column in step f is collected；
H) eluent that step g obtains is concentrated in vacuo to dissolved solids content ＞ 52%～55% of solution；Wherein: vacuum
Degree 0.065Pa～0.09Pa, temperature 55 DEG C～60 DEG C；
I) the concentrated solution vacuum lyophilization obtained in step h is obtained Exocarpium Juglandis Immaturus polyphenol；Its vacuum lyophilization program
As follows:
Drying system vacuum Pa:8 the dry period is≤9.
It is that market is bought that reagent used by the inventive method and instrument are.
The beneficial effects of the present invention is:
1. preparation temperature is low, is not required to first be dried by fresh Exocarpium Juglandis Immaturus and pulverize, it is to avoid conventional decocting method and reflux, extract,
Method needs fresh Exocarpium Juglandis Immaturus is dried and is pulverized, it is to avoid the long-time heating harmful effect to polyphenol in being dried.
2. it is not required to use ethanol or methanol solvate to extract, after fresh Exocarpium Juglandis Immaturus is squeezed the juice, directly divides with AB-8 type resin
From purification Exocarpium Juglandis Immaturus juice, it is to avoid conventional decocting method and reflux extraction need with ethanol or methanol extraction, it is to avoid long in extraction
The time heating harmful effect to polyphenol, it is to avoid consume substantial amounts of organic solvent.
3. using fresh Exocarpium Juglandis Immaturus is raw material, after squeezing the juice and after centrifugal treating, directly utilizes AB-8 type resin and separates pure
Change the polyphenol in Exocarpium Juglandis Immaturus juice, be effectively reduced Exocarpium Juglandis Immaturus and connect for a long time with air and heat in heat drying process
The oxidation touched and occur, fast separating and purifying goes out wherein polyphenol, makes Exocarpium Juglandis Immaturus polyphenol purity bring up to 53% from 9%.
Detailed description of the invention
The method preparing Exocarpium Juglandis Immaturus polyphenol from fresh Exocarpium Juglandis Immaturus used by embodiment is with described in Summary.
It is that market is bought that reagent used by embodiment and instrument are.
Technical scheme, is further described by following embodiment.
Embodiment one:
Fresh Semen Juglandis strips fresh Exocarpium Juglandis Immaturus, and fresh Exocarpium Juglandis Immaturus juice extractor is squeezed the juice, juice in 3000 revs/min,
Centrifugal 20 minutes, separating supernatant liquid and following residue afterwards, the pH value of supernatant liquid is adjusted to 3, mixes, dense with sample solution polyphenol
Degree 2mg/mL, loading volume 1.6BV, loading flow velocity 2BV/h join in its chromatographic column built with 1000 grams of AB-8 type resins,
In chromatographic column, add water, and be washed with water to below chromatographic column after the liquid colorless of outflow, be 65% with volume fraction
Ethanol elution chromatographic column, elution flow rate 1BV/h, elution volume 2.10BV, collect the eluent flowed out below chromatographic column, should
After eluent is concentrated in vacuo to the dissolved solids content 52% of solution when vacuum 0.065Pa, temperature 60 C, vacuum lyophilization
Obtaining Exocarpium Juglandis Immaturus polyphenol, its vacuum lyophilization program is as follows:
Drying system vacuum Pa:8 the dry period is≤9.
Embodiment two:
Fresh Semen Juglandis strips fresh Exocarpium Juglandis Immaturus, and fresh Exocarpium Juglandis Immaturus juice extractor is squeezed the juice, juice in 4500 revs/min,
Centrifugal 10 minutes, separating supernatant liquid and following residue afterwards, the pH value of supernatant liquid is adjusted to 4, mixes, dense with sample solution polyphenol
Degree 3mg/mL, loading volume 1.6BV, loading flow velocity 2BV/h join in its chromatographic column built with 2000 grams of AB-8 type resins,
In chromatographic column, add water, and be washed with water to below chromatographic column after the liquid colorless of outflow, be 70% with volume fraction
Ethanol elution chromatographic column, elution flow rate 2BV/h, elution volume 2.10BV, collect the eluent flowed out below chromatographic column, should
After eluent is concentrated in vacuo to the dissolved solids content 54% of solution when vacuum 0.08Pa, temperature 58 DEG C, vacuum lyophilization
Obtaining Exocarpium Juglandis Immaturus polyphenol, its vacuum lyophilization program is as follows:
Drying system vacuum Pa:8 the dry period is≤9.
Embodiment three:
Fresh Semen Juglandis strips fresh Exocarpium Juglandis Immaturus, and fresh Exocarpium Juglandis Immaturus juice extractor is squeezed the juice, juice in 4000 revs/min,
Centrifugal 15 minutes, separating supernatant liquid and following residue afterwards, the pH value of supernatant liquid is adjusted to 3.6, and mixing, with sample solution polyphenol
Concentration 2.5mg/mL, loading volume 1.6BV, loading flow velocity 2BV/h join its chromatography built with 1500 grams of AB-8 type resins
In post, in chromatographic column add water, and be washed with water to below chromatographic column flow out liquid colorless after, with volume fraction be
The ethanol elution chromatographic column of 75%, elution flow rate 1～2BV/h, elution volume 2.10BV, what collection was flowed out below chromatographic column washes
De-liquid, after this eluent is concentrated in vacuo at vacuum 0.09Pa, temperature 55 DEG C the dissolved solids content 55% of solution, vacuum
Lyophilization obtains Exocarpium Juglandis Immaturus polyphenol, and its vacuum lyophilization program is as follows:
Drying system vacuum Pa:8 the dry period is≤9.
Claims (1)
1. the method preparing Exocarpium Juglandis Immaturus polyphenol from fresh Exocarpium Juglandis Immaturus, it is characterised in that the method comprises the steps:
A) strip fresh Exocarpium Juglandis Immaturus, squeeze the juice with juice extractor；
B) by aforementioned juice in 3000～4500 revs/min, centrifugal 10～20 minutes, supernatant liquid and following residual is separated afterwards
Slag；
C) pH value of supernatant liquid step b obtained is adjusted to 3～4, mixing；
D) solution step c obtained with sample solution polyphenol concentration 2～3mg/mL, sample solution pH3～4, loading volume is
1.6BV, loading flow velocity is that 2BV/h joins in its chromatographic column built with 1000～2000 grams of AB-8 type resins；
E) chromatographic column in step d adds water, be washed with water to the liquid colorless flowed out below chromatographic column；
F) with the chromatographic column in ethanol elution step e that percentage by volume is 65%～75%, elution flow rate 1～2BV/h, eluting
Volume 2.10BV；
G) eluent flowed out below chromatographic column in step f is collected；
H) eluent that step g obtains is concentrated in vacuo to dissolved solids content ＞ 52%～55% of solution；Wherein: vacuum
0.065Pa～0.09Pa, temperature 55 DEG C～60 DEG C；
I) the concentrated solution vacuum lyophilization obtained in step h is obtained Exocarpium Juglandis Immaturus polyphenol；Its vacuum lyophilization program is as follows:
The dry period: 1,2,3,4,5,6,7,8；
Baking temperature DEG C :-50 ,-50 ,-10 ,-5,0,4,10,10；
Drying time h:6,6,6,12,9,4,4,3；
Drying system vacuum Pa:8 the dry period is≤9.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610107933.XA CN105708894A (en) | 2016-02-26 | 2016-02-26 | Method for preparing walnut green husk polyphenol from fresh walnut green husks |
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| CN201610107933.XA CN105708894A (en) | 2016-02-26 | 2016-02-26 | Method for preparing walnut green husk polyphenol from fresh walnut green husks |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107183710A (en) * | 2017-05-09 | 2017-09-22 | 陕西兆信生物科技有限公司 | The method of acidic electrolytic water extraction purification green peel of walnut polyphenol |
| CN107811279A (en) * | 2017-09-25 | 2018-03-20 | 云南中医学院 | A kind of method of medical edible fungal fermentation green peel of walnut and its fermented product and application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101352181A (en) * | 2008-08-15 | 2009-01-28 | 吴桂军 | Method for preparing agent for preventing and treating red spider of Chinese chestnut using extracts from walnut green husk |
| CN101703569A (en) * | 2009-11-06 | 2010-05-12 | 袁小志 | Walnut shell alcohol preparation and applications thereof for preparing medicine treating wart |
-
2016
- 2016-02-26 CN CN201610107933.XA patent/CN105708894A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101352181A (en) * | 2008-08-15 | 2009-01-28 | 吴桂军 | Method for preparing agent for preventing and treating red spider of Chinese chestnut using extracts from walnut green husk |
| CN101703569A (en) * | 2009-11-06 | 2010-05-12 | 袁小志 | Walnut shell alcohol preparation and applications thereof for preparing medicine treating wart |
Non-Patent Citations (1)
| Title |
|---|
| 李琼 等: "大孔吸附树脂分离纯化核桃青皮总多酚", 《食品与机械》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107183710A (en) * | 2017-05-09 | 2017-09-22 | 陕西兆信生物科技有限公司 | The method of acidic electrolytic water extraction purification green peel of walnut polyphenol |
| CN107183710B (en) * | 2017-05-09 | 2020-12-22 | 陕西兆信生物科技有限公司 | Method for extracting and purifying walnut green husk polyphenol by acidic electrolyzed water |
| CN107811279A (en) * | 2017-09-25 | 2018-03-20 | 云南中医学院 | A kind of method of medical edible fungal fermentation green peel of walnut and its fermented product and application |
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Application publication date: 20160629 |