CN109419827A - A kind of extracting method of purslane flavonoid - Google Patents
A kind of extracting method of purslane flavonoid Download PDFInfo
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- CN109419827A CN109419827A CN201710765430.6A CN201710765430A CN109419827A CN 109419827 A CN109419827 A CN 109419827A CN 201710765430 A CN201710765430 A CN 201710765430A CN 109419827 A CN109419827 A CN 109419827A
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- purslane
- water
- eluent
- flavonoid
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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)
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
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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
- A61K2236/33—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
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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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- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
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Abstract
The present invention relates to a kind of extracting methods of purslane flavonoid, belong to the technical field of Natural Medicine Chemistry, the invention is characterised in that using the root of purslane, stem as raw material, it is impregnated with edible ethanol, soxhlet extraction extracts, using grease removal and macroporous adsorption resin chromatography, flavone compound is made.The invention has the advantages that: such compound is green natural product, can be used for pharmacy or food service industry, and the technological process of production is simple, non-environmental-pollution, small investment, easily realizes industrialization.
Description
Technical field
The present invention relates to a kind of extracting methods of purslane flavonoid, belong to the technology neck of Natural Medicine Chemistry
Domain.
Background technique
Purslane also known as five-element's grass, with its Ye Qing, stalk is red, spends Huang, and root is white, and son is black.Purslane (Ye Jihua) is annual
Draft, complete stool are hairless.Purslane can treat various swollen fistulas, after purslane is smashed to pieces, embrocate in affected part.Purslane can disappear
It except abdominal mass, only quenches one's thirst, treats woman's red leukorrhea.Dent dish, which is smashed to pieces, can treat snake skirt-roof.
Flavone compound refers to that basic parent nucleus is the series compound of 2- phenyl chromone, is widely present in plant kingdom,
Many medium-height grass the effective elements of the medicines, it is many kinds of, have multiple biological activities, except with antibacterial, anti-inflammatory, it is disease-resistant become, decompression,
Outside the effects of clearing heat and detoxicating, calm, diuresis, anti-oxidant, anticancer, anti-cancer, inhibit in terms of also have remarkable result, be
A kind of important natural organic oxidation-resistant agent with development prospect.The research trend of flavone compound is medicinal in its in recent years
The exploitation of value is more related to the application study of extraction process, the assay of flavone compound and preparation preparation.
Soxhlet extraction is to extract solid matter can by pure solvent each time using solvent refluxing and siphon principle
It takes, so extraction efficiency is higher.First solid matter should be ground carefully before extraction, soak molten area to increase liquid.Then will consolidate
Body substance is placed in filter paper set, is placed in extraction cell.After solvent ebuillition of heated, steam is risen by gas-guide tube, is condensed
It is instilled in extractor for liquid.When liquid level is more than siphon pipe highest point, i.e., generation siphonage, solution pass back into flask, because
This can extract the moieties for being dissolved in solvent.Solvent refluxing and siphonage are utilized like this, keep the soluble matter in solid rich
Collect in flask.
Summary of the invention
The present invention be directed to the deficiencies in the prior art, it is desirable to provide a kind of high efficiency and selective, easy to operate, yield
It is high, by-product is few, can realization of industrialization the extracting method for preparing purslane flavonoid.
Technical solution of the present invention is carried out according to the following steps:
A. purslane root, stem powder raw material are taken, is fitted into Soxhlet extractor.
B. 60~85% edible ethanols of 3~5 times of material quantities are added, impregnate 20~30 hours, Soxhlet extraction 5~8 is small
When, extracting solution is filtered, ethyl alcohol is recycled in filtrate decompression distillation.
C. after residue is dry, the water of 4~7 times of level of residue is added to dissolve, with the petroleum ether or trichlorine of 3~6 times of level of residue
Methane wash is for several times to colourless.
D. it fetches water and is mutually transferred to large pore resin absorption column, the ratio of raw material and amount of resin is 1: 1.5~3, is first eluted with water, flows through
When the aqueous solution of adsorption column is by light yellow become colorless, takes 0.5~2mL of eluent in 10mL color-comparison tube, add 8~12%
0.03~0.06mL of aluminum nitrate solution, shakes up, and adds 3~6% 0.03~0.06mL of sodium nitrite solution, shakes up, adds 3~6% hydrogen
0.2~0.6mL of sodium hydroxide solution, water are diluted to 5mL, shake up.
E. it is scanned on ultraviolet specrophotometer in 450~550nm wave-length coverage, if continuing to use water without absorption peak
Elution, takes 0.5~2mL of eluent again, scans on ultraviolet specrophotometer with method, until there is absorption peak.
F. it uses the elution of 60~85% edible ethanols instead, receives eluent, eluent becomes rufous from yellow, then becomes yellow
Color, until stop receiving, solvent is evaporated off in 80 DEG C~90 DEG C of water-bath in the eluent received and is precipitated crystal when colourless,
Obtain purslane flavonoid.
Soxhlet extraction extracting described in step b requires to be carried out dehydrating with organic solvent.
The mass ratio of amount of resin described in step c and raw material is 1: 1.5~3.
The present invention has the advantages that
1. the present invention handles raw material using soxhlet extraction, extractant is recycled in soxhlet's extraction device, this was both reduced
Solvent usage, and the operating time is shortened, greatly reduce energy consumption.
The present invention is further illustrated below in conjunction with specific embodiment, but the scope of protection of present invention is not limited to
In following embodiments.
Specific embodiment:
Embodiment 1:
Purslane root, stem powder raw material are taken, is fitted into Soxhlet extractor.60 edible ethanols of 3 times of material quantities, dipping 20 is added
Hour, Soxhlet extraction 5 hours, extracting solution is filtered, ethyl alcohol is recycled in filtrate decompression distillation.After residue is dry, add 4 times of residues
The water of amount dissolves, and wash with the petroleum ether of 3 times of level of residue or chloroform extremely colourless for several times.Water intaking is mutually transferred to macroporous absorption tree
The ratio of rouge column, raw material and amount of resin is 1: 1.5, is first eluted with water, when flowing through the aqueous solution of adsorption column by light yellow become colorless,
It takes eluent 0.5mL in 10mL color-comparison tube, adds 8% aluminum nitrate solution 0.03mL, shake up, add 3% sodium nitrite solution
0.03mL shakes up, and adds 3% sodium hydroxide solution 0.2mL, and water is diluted to 5mL, shakes up.On ultraviolet specrophotometer in 450~
Scanning, if continuing to be eluted with water without absorption peak, takes eluent 0.5mL, with method at ultraviolet point again in 550nm wave-length coverage
It is scanned on light photometer, until there is absorption peak.It uses the elution of 60% edible ethanol instead, receives eluent, eluent is become by yellow
For rufous, then become yellow, until stopping receiving, the eluent received being evaporated off in 80 DEG C of water-bath molten when colourless
Agent precipitates crystal, and obtains purslane flavonoid, yield 70%.
Embodiment 2:
Purslane root, stem powder raw material are taken, is fitted into Soxhlet extractor.60% edible ethanol of 3 times of material quantities is added, impregnates
30 hours, Soxhlet extraction 5 hours, extracting solution is filtered, ethyl alcohol is recycled in filtrate decompression distillation.After residue is dry, add 4 times it is residual
The water of the quantity of slag dissolves, and wash with the petroleum ether of 3 times of level of residue or chloroform extremely colourless for several times.Water intaking is mutually transferred to macroporous absorption
The ratio of resin column, raw material and amount of resin is 1: 3, is first eluted with water, when flowing through the aqueous solution of adsorption column by light yellow become colorless,
It takes eluent 0.5mL in 10mL color-comparison tube, adds 8% aluminum nitrate solution 0.03mL, shake up, add 3~6% sodium nitrites molten
Liquid 0.03mL, shakes up, and adds 3% sodium hydroxide solution 0.2mL, and water is diluted to 5mL, shakes up.In 450 on ultraviolet specrophotometer
Scanning, if continuing to be eluted with water without absorption peak, takes eluent 0.5mL, with method ultraviolet again in~550nm wave-length coverage
It is scanned on spectrophotometer, until there is absorption peak.It uses the elution of 60% edible ethanol instead, receives eluent, eluent is by yellow
Become rufous, then become yellow, until stopping receiving, the eluent received being evaporated off in 80 DEG C of water-bath when colourless
Solvent precipitates crystal, and obtains purslane flavonoid, yield 71%.
Embodiment 3:
Purslane root, stem powder raw material are taken, is fitted into Soxhlet extractor.60~85% edible ethanols of 5 times of material quantities are added,
Dipping 30 hours, Soxhlet extraction 8 hours, extracting solution is filtered, and ethyl alcohol is recycled in filtrate decompression distillation.After residue is dry, add 7 times
It dissolves, wash with the petroleum ether of 6 times of level of residue or chloroform extremely colourless for several times in the water of level of residue.Water intaking is mutually transferred to macropore
The ratio of adsorption resin column, raw material and amount of resin is 1: 3, is first eluted with water, the aqueous solution for flowing through adsorption column becomes nothing from light yellow
It when color, takes eluent 2mL in 10mL color-comparison tube, adds 12% aluminum nitrate solution 0.06mL, shake up, add 6% sodium nitrite
Solution 0.06mL, shakes up, and adds 3~6% sodium hydroxide solution 0.6mL, and water is diluted to 5mL, shakes up.On ultraviolet specrophotometer
It is scanned in 450~550nm wave-length coverage, if continuing to be eluted with water without absorption peak, eluent 2mL is taken again, with method in purple
It is scanned on outer spectrophotometer, until there is absorption peak.It uses the elution of 85% edible ethanol instead, receives eluent, eluent is by Huang
Discoloration is rufous, then becomes yellow, until stopping receiving, the eluent received being steamed in 90 DEG C of water-bath when colourless
Except solvent precipitates crystal, purslane flavonoid, yield 72% are obtained.
Claims (3)
1. a kind of extracting method of purslane flavonoid, it is characterised in that:
A. purslane root, stem powder raw material are taken, is fitted into Soxhlet extractor.
B. 60~85% edible ethanols of 3~5 times of material quantities are added, impregnate 20~30 hours, it Soxhlet extraction 5~8 hours, will
Extracting solution filtering, filtrate decompression distillation, recycles ethyl alcohol.
C. after residue is dry, the water of 4~7 times of level of residue is added to dissolve, with the petroleum ether or chloroform of 3~6 times of level of residue
Washing is for several times to colourless.
D. it fetches water and is mutually transferred to large pore resin absorption column, the ratio of raw material and amount of resin is 1: 1.5~3, is first eluted with water, flows through absorption
It when the aqueous solution of column is by light yellow become colorless, takes 0.5~2mL of eluent in 10mL color-comparison tube, adds 8~12% nitric acid
0.03~0.06mL of aluminum solutions, shakes up, and adds 3~6% 0.03~0.06mL of sodium nitrite solution, shakes up, adds 3~6% hydroxides
0.2~0.6mL of sodium solution, water are diluted to 5mL, shake up.
E. it is scanned on ultraviolet specrophotometer in 450~550nm wave-length coverage, if continuing to be eluted with water without absorption peak,
Again 0.5~2mL of eluent is taken, is scanned on ultraviolet specrophotometer with method, until there is absorption peak.
F. it uses the elution of 60~85% edible ethanols instead, receives eluent, eluent becomes rufous from yellow, then becomes yellow,
Until stopping receiving, solvent being evaporated off in 80 DEG C~90 DEG C of water-bath in the eluent received and is precipitated crystal, is obtained when colourless
Purslane flavonoid.
2. a kind of extracting method of purslane flavonoid according to claim 1, which is characterized in that in step b
The soxhlet extraction extracting requires to be carried out dehydrating with organic solvent.
3. a kind of extracting method of purslane flavonoid according to claim 1, which is characterized in that in step c
The mass ratio of the amount of resin and raw material is 1: 1.5~3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710765430.6A CN109419827A (en) | 2017-08-30 | 2017-08-30 | A kind of extracting method of purslane flavonoid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710765430.6A CN109419827A (en) | 2017-08-30 | 2017-08-30 | A kind of extracting method of purslane flavonoid |
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| Publication Number | Publication Date |
|---|---|
| CN109419827A true CN109419827A (en) | 2019-03-05 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201710765430.6A Pending CN109419827A (en) | 2017-08-30 | 2017-08-30 | A kind of extracting method of purslane flavonoid |
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2017
- 2017-08-30 CN CN201710765430.6A patent/CN109419827A/en active Pending
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Application publication date: 20190305 |