CN107252439A - The extracting method of active component in a kind of walnut - Google Patents
The extracting method of active component in a kind of walnut Download PDFInfo
- Publication number
- CN107252439A CN107252439A CN201710413325.6A CN201710413325A CN107252439A CN 107252439 A CN107252439 A CN 107252439A CN 201710413325 A CN201710413325 A CN 201710413325A CN 107252439 A CN107252439 A CN 107252439A
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- CN
- China
- Prior art keywords
- walnut
- active component
- extracting method
- water
- walnut kernel
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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)
-
- 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
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
-
- 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
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- 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
-
- 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
-
- 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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- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Medicinal Chemistry (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of extracting method of active component in walnut, comprise the following steps:(1) fresh walnut kernel is taken, adds water and is ground to walnut kernel slurries;(2) alcohol steep is added into the walnut kernel slurries, filtered, concentrated, dried, obtain medicinal extract;(3) medicinal extract is dissolved in water, it is 8.0~8.5 to adjust pH, is splined on MCI GEL chromatographic columns, stands, be first eluted with water, then eluted with ethanol solution, collect ethanol eluate, be concentrated and dried, then with acetone solution, crystallized, produce.It is an advantage of the invention that:Process route simple possible, product purity is high, it is easy to industrialized production, with good economic benefit and social benefit.
Description
Technical field
The invention belongs to walnut deep process technology field, the extracting method of active component in more particularly to a kind of walnut.
Background technology
Walnut is containing abundant unrighted acid, albumen in the perennial deciduous tree of Juglandaceae Juglans, walnut kernel
Matter and polyphenol components, the effect with brain tonic and intelligence development and anti-aging.Modern study shows, eats a certain amount of polyphenol to disease
There are prevention and inhibitory action, particularly with good antioxidation activity.
In existing extracting method, polyphenol is extracted from walnut kernel using acetone water, the yield of polyphenol is low, and impurity is more, it is impossible to
Popularization and application are carried out well.
The content of the invention
The present invention proposes a kind of extracting method of active component in walnut, and this method simple possible, gained total polyphenols are pure
Degree is high.
The technical proposal of the invention is realized in this way:
The extracting method of active component, comprises the following steps in a kind of walnut:
(1) fresh walnut kernel is taken, adds water and is ground to walnut kernel slurries;
(2) alcohol steep is added into the walnut kernel slurries, filtered, concentrated, dried, obtain medicinal extract;
(3) medicinal extract is dissolved in water, regulation pH is 8.0~8.5, is splined on MCI GEL chromatographic columns, stands, first uses
Water elution, then eluted with ethanol solution, ethanol eluate is collected, is concentrated and dried, then with acetone solution, crystallizes, produces.
Preferably, the amount added water in the step (1) is 0.2~1 times of weight of the fresh walnut kernel weight.
Preferably, the addition of ethanol is 3~10 times of weight of the walnut kernel slurry weight in the step (2).
Preferably, the temperature of extraction is 15 DEG C~20 DEG C in the step (2), the number of times of extraction is 1~5 time, every time
The time of extraction is 1~5 hour.
Preferably, the time stood in the step (3) is 1~2 hour.
Preferably, the ethanol solution that ethanol solution is eluted in the step (3) is mass percent concentration is 40%~
70% ethanol water.
Preferably, MCI GEL chromatographic columns are selected from MCI GEL CHP20Y in the step (3).
Compared with prior art, the beneficial effects of the invention are as follows:
Walnut kernel is first subjected to alcohol extracting, crude extract is obtained, MCI GEL chromatographic columns, second are splined under the conditions of weakly alkaline
Alcohol is eluted, then is refined through acetone crystallization.This method process route simple possible, products obtained therefrom purity is high, it is easy to industrialize
Big production, with good economic benefit and social benefit.
Embodiment
The technical scheme in the present invention is clearly and completely described below, it is clear that described embodiment is only
Several embodiments therein of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, the common skill in this area
The every other embodiment that art personnel are obtained under the premise of creative work is not made, belongs to the model that the present invention is protected
Enclose.
Embodiment 1
The extracting method of active component, comprises the following steps in a kind of walnut:
(1) fresh walnut kernel, plus the water of 0.8 times of weight is taken to be ground to walnut kernel slurries;
(2) ethanol that the mass percent concentration that 6 times of weight is added into the walnut kernel slurries is 95% is at 15 DEG C
Under the conditions of extract 3 times, the time extracted every time be 3 hours, filter, concentrate, dry, obtain medicinal extract;
(3) suitable quantity of water is added to dissolve the medicinal extract, regulation pH is 8.2, is splined on MCI GEL CHP20Y chromatographic columns, is stood
1.5 hours, first it is eluted with water, then is eluted with mass percent concentration for 60% ethanol solution, collects ethanol eluate, concentration
Dry, then with acetone solution, crystallize, obtain the walnut polyphenol that purity is 96.3%.
Embodiment 2
The extracting method of active component, comprises the following steps in a kind of walnut:
(1) fresh walnut kernel, plus the water of 1 times of weight is taken to be ground to walnut kernel slurries;
(2) ethanol that the mass percent concentration that 10 times of weight is added into the walnut kernel slurries is 95% is at 20 DEG C
Under the conditions of extract 5 times, the time extracted every time be 5 hours, filter, concentrate, dry, obtain medicinal extract;
(3) suitable quantity of water is added to dissolve the medicinal extract, regulation pH is 8.5, is splined on MCI GEL CHP20Y chromatographic columns, is stood
2 hours, first it is eluted with water, then is eluted with mass percent concentration for 70% ethanol solution, collect ethanol eluate, concentration is dry
It is dry, then with acetone solution, crystallize, obtain the walnut polyphenol that purity is 95.7%.
Embodiment 3
The extracting method of active component, comprises the following steps in a kind of walnut:
(1) fresh walnut kernel, plus the water of 0.2 times of weight is taken to be ground to walnut kernel slurries;
(2) ethanol that the mass percent concentration that 3 times of weight is added into the walnut kernel slurries is 90% is at 15 DEG C
Under the conditions of extract 1 time, the time extracted every time be 1 hour, filter, concentrate, dry, obtain medicinal extract;
(3) suitable quantity of water is added to dissolve the medicinal extract, regulation pH is 8.0, is splined on MCI GEL CHP20Y chromatographic columns, is stood
1 hour, first it is eluted with water, then is eluted with mass percent concentration for 40% ethanol solution, collect ethanol eluate, concentration is dry
It is dry, then with acetone solution, crystallize, obtain the walnut polyphenol that purity is 95.1%.
Embodiment 4
The extracting method of active component, comprises the following steps in a kind of walnut:
(1) fresh walnut kernel, plus the water of 0.4 times of weight is taken to be ground to walnut kernel slurries;
(2) ethanol that the mass percent concentration that 8 times of weight is added into the walnut kernel slurries is 95% is at 18 DEG C
Under the conditions of extract 2 times, the time extracted every time be 2 hours, filter, concentrate, dry, obtain medicinal extract;
(3) suitable quantity of water is added to dissolve the medicinal extract, regulation pH is 8.1, is splined on MCI GEL CHP20Y chromatographic columns, is stood
2 hours, first it is eluted with water, then is eluted with mass percent concentration for 50% ethanol solution, collect ethanol eluate, concentration is dry
It is dry, then with acetone solution, crystallize, obtain the walnut polyphenol that purity is 95.8%.
Embodiment 5
The extracting method of active component, comprises the following steps in a kind of walnut:
(1) fresh walnut kernel, plus the water of 0.8 times of weight is taken to be ground to walnut kernel slurries;
(2) ethanol that the mass percent concentration that 4 times of weight is added into the walnut kernel slurries is 90% is at 16 DEG C
Under the conditions of extract 4 times, the time extracted every time be 4 hours, filter, concentrate, dry, obtain medicinal extract;
(3) suitable quantity of water is added to dissolve the medicinal extract, regulation pH is 8.0, is splined on MCI GEL CHP20Y chromatographic columns, is stood
2 hours, first it is eluted with water, then is eluted with mass percent concentration for 50% ethanol solution, collect ethanol eluate, concentration is dry
It is dry, then with acetone solution, crystallize, obtain the walnut polyphenol that purity is 96.2%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God is with principle, and any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.
Claims (7)
1. the extracting method of active component in a kind of walnut, it is characterised in that:Comprise the following steps:
(1) fresh walnut kernel is taken, adds water and is ground to walnut kernel slurries;
(2) alcohol steep is added into the walnut kernel slurries, filtered, concentrated, dried, obtain medicinal extract;
(3) medicinal extract is dissolved in water, regulation pH is 8.0~8.5, is splined on MCI GEL chromatographic columns, stands, is first washed with water
It is de-, then eluted with ethanol solution, ethanol eluate is collected, is concentrated and dried, then with acetone solution, crystallizes, produces.
2. the extracting method of active component in a kind of walnut according to claim 1, it is characterised in that:The step (1)
In the amount that adds water be the fresh walnut kernel weight 0.2~1 times of weight.
3. the extracting method of active component in a kind of walnut according to claim 1, it is characterised in that:The step (2)
The addition of middle ethanol is 3~10 times of weight of the walnut kernel slurry weight.
4. the extracting method of active component in a kind of walnut according to claim 1, it is characterised in that:The step (2)
The temperature of middle extraction is 15 DEG C~20 DEG C, and the number of times of extraction is 1~5 time, and the time extracted every time is 1~5 hour.
5. the extracting method of active component in a kind of walnut according to claim 1, it is characterised in that:The step (3)
The time of middle standing is 1~2 hour.
6. the extracting method of active component in a kind of walnut according to claim 1, it is characterised in that:The step (3)
The ethanol solution of middle ethanol solution elution is the ethanol water that mass percent concentration is 40%~70%.
7. the extracting method of active component in a kind of walnut according to claim 1, it is characterised in that:The step (3)
Middle MCI GEL chromatographic columns are selected from MCI GEL CHP20Y.
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CN201710413325.6A CN107252439A (en) | 2017-06-05 | 2017-06-05 | The extracting method of active component in a kind of walnut |
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CN201710413325.6A CN107252439A (en) | 2017-06-05 | 2017-06-05 | The extracting method of active component in a kind of walnut |
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CN201710413325.6A Pending CN107252439A (en) | 2017-06-05 | 2017-06-05 | The extracting method of active component in a kind of walnut |
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2008074807A (en) * | 2006-09-25 | 2008-04-03 | Oriza Yuka Kk | Hepatoprotector |
EP1789065B1 (en) * | 2004-08-06 | 2012-11-21 | Bio-Quant, Inc. | Process for preparing an anti-microbial fraction from juglans regia |
-
2017
- 2017-06-05 CN CN201710413325.6A patent/CN107252439A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1789065B1 (en) * | 2004-08-06 | 2012-11-21 | Bio-Quant, Inc. | Process for preparing an anti-microbial fraction from juglans regia |
JP2008074807A (en) * | 2006-09-25 | 2008-04-03 | Oriza Yuka Kk | Hepatoprotector |
Non-Patent Citations (3)
Title |
---|
李丹等: "核桃仁中鞣质成分的提取工艺研究", 《黑龙江医药》 * |
白长财: "MCI资料大全-MCI柱以及MCI填料", 《HTTPS://WENKU.BAIDU.COM/VIEW/479CBFBE76A20029BD642D8C.HTML》 * |
金哲雄: "核桃仁可水解丹宁成分研究Ⅱ", 《中国中药杂志》 * |
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