CN107311850A - A kind of method that juglone is prepared from green peel of walnut - Google Patents
A kind of method that juglone is prepared from green peel of walnut Download PDFInfo
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- CN107311850A CN107311850A CN201710413322.2A CN201710413322A CN107311850A CN 107311850 A CN107311850 A CN 107311850A CN 201710413322 A CN201710413322 A CN 201710413322A CN 107311850 A CN107311850 A CN 107311850A
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- walnut
- green peel
- juglone
- water
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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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- Organic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a kind of method that juglone is prepared from green peel of walnut, comprise the following steps：(1) it is particle to take green peel of walnut to crush, and small fire is fried to micro- Huang, adds the vexed profit of watery hydrochloric acid, then small fire is fried 45~60 minutes again, obtains rascal parched medicinal material；(2) the rascal parched medicinal material is extracted with water, filtered, concentration obtains medicinal extract；(3) medicinal extract is dissolved in water, is splined on MCI GEL chromatographic columns, stood, be first eluted with water, then eluted with ethanol solution, collect ethanol eluate, be concentrated and dried, again with methanol dissolving, crystallization is produced.It is an advantage of the invention that：Process route simple possible, can extract effectively from green peel of walnut and isolate juglone, and products obtained therefrom 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, more particularly to a kind of side that juglone is prepared from green peel of walnut
Method.
Background technology
Green peel of walnut, the entitled pericarpium juglandis of Chinese medicine is the thick green pericarp of a thickness outside walnut, and gas is micro-, mildly bitter flavor.I
State produces 450000 tons or so of green peel of walnut per year, only has small part, most green peel of walnut for medicinal green peel of walnut every year
All cause to waste as discarded object.
Modern study shows, contain in green peel of walnut juglone, tannin, gallic acid with antitumor action etc. into
Point, because English walnut quinone content is low (about 0.03~3mg/g), separation difficulty is extracted, it is necessary to further be studied.
The content of the invention
The present invention proposes a kind of method that juglone can be effectively prepared from green peel of walnut.
The technical proposal of the invention is realized in this way：
A kind of method that juglone is prepared from green peel of walnut, comprises the following steps：
(1) it is particle to take green peel of walnut to crush, and small fire is fried to micro- Huang, adds the vexed profit of watery hydrochloric acid, then again small fire stir-fry 45~
60 minutes, obtain rascal parched medicinal material；
(2) the rascal parched medicinal material is extracted with water, filtered, concentration obtains medicinal extract；
(3) medicinal extract is dissolved in water, is splined on MCI GEL chromatographic columns, stood, be first eluted with water, then it is molten with ethanol
Liquid is eluted, and collects ethanol eluate, is concentrated and dried, and again with methanol dissolving, crystallization is produced.
Specifically, MCI GEL chromatographic columns can be MCI GEL CHP20P.
Preferably, watery hydrochloric acid is the aqueous hydrochloric acid solution that mass percent concentration is 1%~5% in the step (1).
Preferably, extracting by the way of decocting to carry out in the step (2), the number of times of extraction is 1~5 time, often
The time of secondary extraction is 1~5 hour.
Preferably, the time stood in the step (3) is 1~2 hour.
Preferably, ethanol solution is the ethanol water of mass percent concentration 70%~95% in the step (3).
The temperature of small fire is 40 DEG C~70 DEG C in the present invention.
Compared with prior art, the beneficial effects of the invention are as follows：
First by the green peel of walnut vexed profit of watery hydrochloric acid, then with water extraction, MCI GEL chromatographic columns are splined on, remove water elution, receive
Collect ethanol eluate, after concentrate drying, with methanol crystallization, process route simple possible can be extracted effectively from green peel of walnut and divided
Juglone is separated out, products obtained therefrom purity is high, it is easy to industrialized 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
A kind of method that juglone is prepared from green peel of walnut, comprises the following steps：
(1) it is particle to take green peel of walnut to crush, and small fire is fried to micro- Huang, adds the hydrochloric acid water that mass percent concentration is 3%
The vexed profit of solution, then small fire is fried 50 minutes again, obtains rascal parched medicinal material；
(2) the rascal parched medicinal material is extracted with water, filtered, concentration obtains medicinal extract；Extract by the way of decocting
OK, the number of times of extraction is 3 times, and the time extracted every time is 3 hours.
(3) medicinal extract is dissolved in water, is splined on MCI GEL chromatographic columns, stood 1.5 hours, be first eluted with water, then use
The ethanol water elution of mass percent concentration 90%, collects ethanol eluate, is concentrated and dried, again with methanol dissolving, crystallization,
Produce.
After testing, the rate of recovery of juglone is 71.53% in green peel of walnut, and products obtained therefrom purity is 78.34%.
Embodiment 2
A kind of method that juglone is prepared from green peel of walnut, comprises the following steps：
(1) it is particle to take green peel of walnut to crush, and small fire is fried to micro- Huang, adds the hydrochloric acid water that mass percent concentration is 5%
The vexed profit of solution, then small fire is fried 60 minutes again, obtains rascal parched medicinal material；
(2) the rascal parched medicinal material is extracted with water, filtered, concentration obtains medicinal extract；Extract by the way of decocting
OK, the number of times of extraction is 5 times, and the time extracted every time is 5 hours.
(3) medicinal extract is dissolved in water, is splined on MCI GEL chromatographic columns, stood 2 hours, be first eluted with water, then use matter
The ethanol water elution of percent concentration 95% is measured, ethanol eluate is collected, is concentrated and dried, again with methanol dissolving, crystallization, i.e.,
.
After testing, the rate of recovery of juglone is 70.16% in green peel of walnut, and products obtained therefrom purity is 77.37%.
Embodiment 3
A kind of method that juglone is prepared from green peel of walnut, comprises the following steps：
(1) it is particle to take green peel of walnut to crush, and small fire is fried to micro- Huang, adds the hydrochloric acid water that mass percent concentration is 1%
The vexed profit of solution, then small fire is fried 45 minutes again, obtains rascal parched medicinal material；
(2) the rascal parched medicinal material is extracted with water, filtered, concentration obtains medicinal extract；Extract by the way of decocting
OK, the number of times of extraction is 1 time, and the time extracted every time is 1 hour.
(3) medicinal extract is dissolved in water, is splined on MCI GEL chromatographic columns, stood 1 hour, be first eluted with water, then use matter
The ethanol water elution of percent concentration 70% is measured, ethanol eluate is collected, is concentrated and dried, again with methanol dissolving, crystallization, i.e.,
.
After testing, the rate of recovery of juglone is 70.64% in green peel of walnut, and products obtained therefrom purity is 78.09%.
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 (5)
1. a kind of method that juglone is prepared from green peel of walnut, it is characterised in that：Comprise the following steps：
(1) it is particle to take green peel of walnut to crush, and small fire is fried to micro- Huang, adds the vexed profit of watery hydrochloric acid, then small fire fries 45~60 points again
Clock, obtains rascal parched medicinal material；
(2) the rascal parched medicinal material is extracted with water, filtered, concentration obtains medicinal extract；
(3) medicinal extract is dissolved in water, is splined on MCI GEL chromatographic columns, stood, be first eluted with water, then washed with ethanol solution
It is de-, ethanol eluate is collected, is concentrated and dried, again with methanol dissolving, crystallization is produced.
2. a kind of method that juglone is prepared from green peel of walnut according to claim 1, it is characterised in that：The step
(1) watery hydrochloric acid is the aqueous hydrochloric acid solution that mass percent concentration is 1%~5% in.
3. a kind of method that juglone is prepared from green peel of walnut according to claim 1, it is characterised in that：The step
(2) extract by the way of decocting to carry out in, the number of times of extraction is 1~5 time, and the time extracted every time is 1~5 hour.
4. a kind of method that juglone is prepared from green peel of walnut according to claim 1, it is characterised in that：The step
(3) time stood in is 1~2 hour.
5. a kind of method that juglone is prepared from green peel of walnut according to claim 1, it is characterised in that：The step
(3) ethanol solution is the ethanol water of mass percent concentration 70%~95% in.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710413322.2A CN107311850A (en) | 2017-06-05 | 2017-06-05 | A kind of method that juglone is prepared from green peel of walnut |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710413322.2A CN107311850A (en) | 2017-06-05 | 2017-06-05 | A kind of method that juglone is prepared from green peel of walnut |
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| CN107311850A true CN107311850A (en) | 2017-11-03 |
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| CN201710413322.2A Pending CN107311850A (en) | 2017-06-05 | 2017-06-05 | A kind of method that juglone is prepared from green peel of walnut |
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Cited By (3)
| 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 |
| CN111454587A (en) * | 2020-04-24 | 2020-07-28 | 杭州彩润科技有限公司 | Comprehensive processing and utilizing method for dyeing of pericarpium juglandis |
| CN113416128A (en) * | 2021-07-07 | 2021-09-21 | 吕梁学院 | Method for separating and purifying juglone in walnut shells |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1931816A (en) * | 2006-10-11 | 2007-03-21 | 东北林业大学 | Juglone extracting process |
| CN101906030A (en) * | 2010-08-23 | 2010-12-08 | 河北理工大学 | Method for extracting juglone from walnut green husk residue by microwave reflux |
-
2017
- 2017-06-05 CN CN201710413322.2A patent/CN107311850A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1931816A (en) * | 2006-10-11 | 2007-03-21 | 东北林业大学 | Juglone extracting process |
| CN101906030A (en) * | 2010-08-23 | 2010-12-08 | 河北理工大学 | Method for extracting juglone from walnut green husk residue by microwave reflux |
Non-Patent Citations (3)
| Title |
|---|
| 仲军梅: "核桃青皮色素活性成分提取及其应用", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
| 马乐 等: "大孔树脂对核桃青皮中胡桃醌的分离纯化", 《食品与发酵工业》 * |
| 魏赫楠 等: "核桃青皮中胡桃醌的提取工艺", 《江苏农业科学》 * |
Cited By (4)
| 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 |
| CN111454587A (en) * | 2020-04-24 | 2020-07-28 | 杭州彩润科技有限公司 | Comprehensive processing and utilizing method for dyeing of pericarpium juglandis |
| CN111454587B (en) * | 2020-04-24 | 2021-07-13 | 杭州彩润科技有限公司 | Comprehensive processing and utilizing method for dyeing of pericarpium juglandis |
| CN113416128A (en) * | 2021-07-07 | 2021-09-21 | 吕梁学院 | Method for separating and purifying juglone in walnut shells |
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Application publication date: 20171103 |
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