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 PDF

Info

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
Authority
CN
China
Prior art keywords
walnut
active component
extracting method
water
walnut kernel
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.)
Pending
Application number
CN201710413325.6A
Other languages
Chinese (zh)
Inventor
张跃进
杨文�
黄翔
段学荣
郭璐璐
李柯桦
刘思严
尹文剑
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yunnan Moer Garden Biological Science & Technology Development Co Ltd
Original Assignee
Yunnan Moer Garden Biological Science & Technology Development Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Yunnan Moer Garden Biological Science & Technology Development Co Ltd filed Critical Yunnan Moer Garden Biological Science & Technology Development Co Ltd
Priority to CN201710413325.6A priority Critical patent/CN107252439A/en
Publication of CN107252439A publication Critical patent/CN107252439A/en
Pending legal-status Critical Current

Links

Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/52Juglandaceae (Walnut family)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/55Liquid-liquid separation; Phase separation

Landscapes

  • 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

The extracting method of active component in a kind of walnut
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.
CN201710413325.6A 2017-06-05 2017-06-05 The extracting method of active component in a kind of walnut Pending CN107252439A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710413325.6A CN107252439A (en) 2017-06-05 2017-06-05 The extracting method of active component in a kind of walnut

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710413325.6A CN107252439A (en) 2017-06-05 2017-06-05 The extracting method of active component in a kind of walnut

Publications (1)

Publication Number Publication Date
CN107252439A true CN107252439A (en) 2017-10-17

Family

ID=60023907

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710413325.6A Pending CN107252439A (en) 2017-06-05 2017-06-05 The extracting method of active component in a kind of walnut

Country Status (1)

Country Link
CN (1) CN107252439A (en)

Citations (2)

* Cited by examiner, † Cited by third party
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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》 *

Similar Documents

Publication Publication Date Title
CN102718668B (en) Method for extracting synephrine and hesperidin from citrus aurantium
CN102701914B (en) Method for extracting hydroxytyrosol from olive leaves
CN106220698A (en) A kind of method of separating high-purity Hesperidin, neohesperidin, naringin and Neosynephrine from Fructus Aurantii Immaturus
CN102993154A (en) Method for extracting purple sweet potato anthocyanin
CN103554076A (en) Method for rapidly extracting high-purity dihydromyricetin in ampelopsis grossedentata leaves
CN105111098A (en) Method for extracting and purifying monomeric macamide compounds from maca
CN102351936A (en) Method for extracting ecdysterone from plant
CN102603699A (en) Method for extracting epigallocatechin gallate from oil-tea-cake
CN103044442B (en) A kind of method of separation and purification GA, GB and bilobalide from Folium Ginkgo extract
CN103059092B (en) A kind of method extracting Oleanolic Acid from pawpaw
CN111057117A (en) Comprehensive utilization method of immature bitter oranges
JP7083920B2 (en) Cytisinicline isolation method
CN107252439A (en) The extracting method of active component in a kind of walnut
CN110819444A (en) Method for extracting tea oil and tea saponin from camellia seeds
CN102659760B (en) Extraction technology of nicotine by acid process
CN112500448B (en) Method for extracting laxogenin from Liliaceae Allium plant
CN102731598A (en) Comprehensive utilization method of dried orange peel strips
CN108047288B (en) Preparation method of geniposide
CN102285976A (en) Method for extracting isoorientin from bamboo leaf flavones
CN105085587A (en) Extraction and purification process method for forsythiaside A in fructus forsythiae leaves
CN102603852A (en) Preparation method of tripterine
CN103613575A (en) Method for purifying high-content epigallocatechin gallate (EGCG)
CN106316797A (en) Method for preparing hydroxytyrosol by using immobilized enzymic method coupled film technique
CN102432660A (en) Extraction and separation method of cyclocarioside I
CN106889539A (en) A kind of method that utilization aqueous extraction-alcohol precipitation technology extracts honeycomb element from honeycomb

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20171017

RJ01 Rejection of invention patent application after publication