CN1709542A - Method for extracting flavone substance from leaves of Diospyms kaki by double water-phase extraction - Google Patents
Method for extracting flavone substance from leaves of Diospyms kaki by double water-phase extraction Download PDFInfo
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- CN1709542A CN1709542A CN 200410026240 CN200410026240A CN1709542A CN 1709542 A CN1709542 A CN 1709542A CN 200410026240 CN200410026240 CN 200410026240 CN 200410026240 A CN200410026240 A CN 200410026240A CN 1709542 A CN1709542 A CN 1709542A
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- persimmon leaf
- aqueous
- leaf flavone
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Abstract
The present invention relates to a method to extract persimmon leaf flavone. The technical character is: drying the persimmon leaf and crushing; adding ethanol liquor and soaking; filtrating ;we get coarse liquor; get part of said liquor, add PEG polymer and ammonia sulfate, mix well-proportioned and it is divided to up and down two parts. Get the part of up part which contains polyglycol polymer, add water, acetic acid grease and inorganic salt and mix well-proportioned. Get the part of acetic acid grease, decompress, distill and concentrate the liquor; Get it in vacuum and we will get the solid persimmon leaf flavone. This method can increase the rate of extracting and get high-grade persimmon leaf flavone. Meanwhile the method is economic and simple.
Description
Technical field
The present invention relates to the method that a kind of aqueous two-phase extraction extracts persimmon leaf flavone class material.
Background technology: the persimmon leaf is the fresh or dry blade of persimmon.Be stated from bright " the southern regions of the Yunnan Province book on Chinese herbal medicine " as the medicinal beginning, say: " applying ulcer on the shank " through red leaves.How on the books later all families book on Chinese herbal medicine and doctor's (medicine) book be also.Its bitter, acid, puckery, cool in nature, have removing heat from the lung to relieve cough, cooling blood and hemostasis, effect promoting blood circulation and removing blood stasis, hypotensive.Be mainly used in cough breathe heavily, illness such as pulmonary emphysema, various internal haemorrhage, hypertension.Main active ingredient in the persimmon leaf is flavones.The flavone compound of having found at present has the Radix Astragali, isoquercitin, kaempferol, Quercetin etc.Studies show that both at home and abroad: persimmon leaf flavone has antihypertensive function and promotes plant growth effect, is a kind of crop, melon and fruit volume increase agent and up-and-coming natural hypotensor with practical value.
Flavones mainly exists with the glucoside form in the persimmon leaf, and water, methyl alcohol, the ethanol waters of adopting are made solvent more when generally extracting, and make extractant with ethyl acetate.According to another report, the someone adopts water to carry the method extraction separation persimmon leaf flavone compounds of resin absorption.All there is following problem in these methods: complex operation, recovery rate is lower.
Summary of the invention
The technical problem that solves
For fear of the deficiencies in the prior art part, the invention provides the method that a kind of aqueous two-phase extraction extracts persimmon leaf flavone class material, utilize the characteristics of aqueous two phase extraction technique, not only improved the recovery rate that extracts persimmon leaf flavone class material, and can obtain high-quality Flavonoid substances, while method itself is economy but also simple to operate not only.
Technical scheme
Adopt the method for aqueous two-phase extraction persimmon leaf flavone class material in the present invention,
The characteristics of aqueous two phase extraction technique have:
(1) nearly 75%～99%, two interfacial tensions are extremely low for the water content of system, and the biologically active of composition and border quality transmission mutually help to remain valid;
(2) upper and lower phase density is little, and general 10
-2Gcm
-3About, be one of percentage of water density;
(3) the phase-splitting time is short;
(4) aqueous two-phase extraction is easy to continued operation, engineering is amplified, and can directly linearly amplify 40,000 times;
(5) the aqueous two-phase extraction treating capacity is big, and energy consumption is low; Prime cost consumes in the use of polymer, and polymer can recycle, and therefore, production cost is lower.
Technical characterictic of the present invention is:
A, solid-liquid leaching: with the oven dry of persimmon leaf, pulverizing, add ethanolic solution, solid-liquid leaching obtains persimmon leaf crude extract behind the filtering and impurity removing;
B, aqueous two-phase extraction: get above-mentioned persimmon leaf crude extract, add PEG polymer and ammonium sulfate aqueous two-phase system, mixing, be divided into upper and lower two-phase, 15 ℃～30 ℃ of phase separation temperature, the time is 2～6 hours;
C, acetate esters back extraction: take out the last phase that is rich in polyethylene glycol polymer, add water, acetate esters and inorganic salts, mixing, system at room temperature leaves standstill and is divided into upper and lower two-phase, and phase separation temperature is a room temperature, and the time is 1～3 hour.
D, decompression distillation, vacuum drying: take out the phase of the acetate esters that contains a large amount of Flavonoid substances, it is carried out decompression distillation, concentrated solution, then this concentrate is carried out vacuum drying, obtain solid persimmon leaf flavone class material.
In above-mentioned aqueous two-phase extraction, can also add inorganic salts when adding PEG polymer and ammonium sulfate aqueous two-phase system, inorganic salts can be NaCl or Na
2SO
4
The PEG polymer of above-mentioned adding is 5%～25%, and ammonium sulfate is 10%～20%, and wherein the molecular weight of PEG polymer is 300～1500.
The acetate esters of above-mentioned adding can be butyl acetate or ethyl acetate.
Beneficial effect
The invention has the beneficial effects as follows:
(1) phase-splitting is rapid
In experiment, observe, adopt the aqueous two-phase extraction method, got final product phase-splitting in about about 20 minutes, and do not have emulsion layer, shortened experimental period.
(2) process integration
Aqueous two-phase extraction had both reached pretreated purpose, had concentrated feed liquid again.Show as a large amount of impurity (as hydroaropic substance, cell fragment etc.) and enter down phase, Flavonoid substances enters phase, on compare original treatment fluid and greatly reduce, cycles of concentration has reached more than 4 times;
(3) the inventive method is simple, is easy to grasp, and is not affected by environment, instant effect.
Description of drawings
The present invention will be further described below in conjunction with drawings and Examples.
Fig. 1: process flow diagram
The specific embodiment
Now in conjunction with the accompanying drawings the present invention is further described:
Embodiment 1:
(1) solid-liquid leaching
Take by weighing the persimmon leaf 20g through cleaning, impurity elimination, oven dry, pulverizing, add the 50% ethanol 300mL lixiviate 3h that refluxes, distillating recovering solvent with last extracting liquid filtering removal of impurities, obtains filtrate 153g.
(2) aqueous two-phase extraction
Get above-mentioned filtrate, add 20g polyethylene glycol, 35g (NH
4)
2SO
4, 100g water, add inorganic salts NaCl 5g mixing again, at 15 ℃ of phase-splitting 2h～6h.
(3) butyl acetate or ethyl acetate back extraction
The last phase 124mL of polyethylene glycol polymer is rich in taking-up, add water 50mL, 80mL butyl acetate or ethyl acetate and 3gNaCl, fully mixing, system at room temperature leaves standstill phase-splitting 1h～3h to thoroughly being divided into upper and lower two-phase, and the butyl acetate that contains a large amount of Flavonoid substances is treated each other further processing.
(4) decompression distillation, vacuum drying
Take out butyl acetate phase 102mL and carry out the decompression distillation concentrated solution, concentrate is placed 60 ℃～80 ℃ following vacuum drying, obtain solid persimmon leaf flavone class material.
Embodiment 2
(1) solid-liquid leaching
Take by weighing through cleaning the persimmon leaf 20g of impurity elimination, oven dry, pulverizing, add 70% ethanol 400mL backflow lixiviate 5h, distillating recovering solvent with last extracting liquid filtering removal of impurities, obtains filtrate 190g.
(2) aqueous two-phase extraction
Get above-mentioned filtrate, add 25g polyethylene glycol, 45g (NH
4)
2SO
4, 95g water, add 2g NaCl again, mixing is at 25 ℃ of phase-splitting 2h～6h.
(3) butyl acetate or ethyl acetate back extraction
The last phase 186mL of polyethylene glycol polymer is rich in taking-up, adds water 75mL, the 113mL butyl acetate, 3g NaCl, abundant mixing, system at room temperature leaves standstill phase-splitting 1h～3h to thoroughly being divided into upper and lower two-phase, and the butyl acetate that contains a large amount of Flavonoid substances is treated each other further processing.
(4) decompression distillation, vacuum drying
Above-mentioned butyl acetate or ethyl acetate are carried out decompression distillation mutually come concentrated solution, concentrate is placed 60 ℃～80 ℃ following vacuum drying, obtain solid persimmon leaf flavone class material.
Embodiment 3
(1) solid-liquid leaching
Take by weighing through cleaning the persimmon leaf 20g of impurity elimination, oven dry, pulverizing, add 60% ethanol 500mL backflow lixiviate 8h, distillating recovering solvent with last extracting liquid filtering removal of impurities, obtains filtrate 389g.
(2) aqueous two-phase extraction
Get above-mentioned filtrate, add 35g polyethylene glycol, 65g (NH
4)
2SO
4, 125g water, add inorganic salts 3g NaCl again, mixing is at 30 ℃ of phase-splitting 2h～6h.
(3) butyl acetate or ethyl acetate back extraction
The last phase 221mL of polyethylene glycol polymer is rich in taking-up, adds water 85mL, the 126mL butyl acetate, 3g NaCl, abundant mixing, system at room temperature leaves standstill phase-splitting 1h～3h to thoroughly being divided into upper and lower two-phase, and the butyl acetate that contains a large amount of Flavonoid substances is treated each other further processing.
(4) decompression distillation, vacuum drying
Take out butyl acetate phase 238mL and carry out the decompression distillation concentrated solution, concentrate is placed 60 ℃～80 ℃ following vacuum drying, obtain solid persimmon leaf flavone class material.
Products obtained therefrom is pressed the Chinese Pharmacopoeia standard detection, and contained persimmon leaf flavone compounds is about 12.1% (AAS) in the product.
The present invention is based on following discovery: the very big symmetry that persimmon leaf flavone class material distributes in PEG/ ammonium sulfate aqueous two-phase system.Table 1 has provided the distribute data of persimmon leaf flavone class material in PEG/ ammonium sulfate aqueous two-phase.The principle of double-aqueous phase system extraction and separation technology is: the selectivity of persimmon leaf flavone class material in double-aqueous phase system distributed.After persimmon leaf flavone class material enters double-aqueous phase system, between upper and lower phase, carry out selectivity and distribute, show certain distribution coefficient.Persimmon leaf flavone class material has certain compatibility to PEG, make persimmon leaf flavone class material can be easier to be dissolved in the last phase that is rich in PEG, and some impurity are distributed in down phase, and the distribution coefficient of persimmon leaf flavone class material is generally greater than 16, and extraction yield is between 78.9%～94.7%.
The distribution behavior of table 1 persimmon leaf flavone class material in PEG/ ammonium sulfate aqueous two-phase system
| Sequence number | Total %wt PEG (NH that forms 4) 2SO 4 | Compare (R) | Distribution coefficient (K) | Extraction yield % (Y) |
| ?1 | ?10????9 | ?0.354 | ?16.0 | ?78.9 |
| ?2 | ?10????11 | ?0.332 | ?39.8 | ?84.2 |
| ?3 | ?10????13 | ?0.276 | ?67.6 | ?86.9 |
| ?4 | ?10????15 | ?0.257 | ?84.5 | ?92.1 |
| ?5 | ?10????17 | ?0.249 | ?94.7 | ?94.7 |
In the table: compare R=V
t/ V
b
Distribution coefficient K=C
t/ C
b
Extraction yield Y=V
tC
t/ (V
tC
t+ V
bC
b)
In the formula: V
t, V
bThe volume of-upper and lower phase;
C
t, C
b-persimmon leaf flavone compounds is in upper and lower concentration in mutually;
Therefore,, persimmon leaf flavone class material is concentrated and purify, finally obtain the finished product of persimmon leaf flavone class material through the processing of processes such as above-mentioned solid-liquid leaching, the extraction of PEG/ ammonium sulfate aqueous two-phase system, organic solvent back extraction.
Claims (9)
1, a kind of aqueous two-phase extraction extracts the method for persimmon leaf flavone class material, it is characterized in that:
A, solid-liquid leaching: with the oven dry of persimmon leaf, pulverizing, add ethanolic solution, solid-liquid leaching obtains persimmon leaf crude extract behind the filtering and impurity removing;
B, aqueous two-phase extraction: get above-mentioned persimmon leaf crude extract, add PEG polymer and ammonium sulfate aqueous two-phase system, mixing, be divided into upper and lower two-phase;
C, acetate esters back extraction: take out the last phase that is rich in polyethylene glycol polymer, add water, acetate esters and inorganic salts, mixing, system at room temperature leaves standstill and is divided into upper and lower two-phase;
D, decompression distillation, vacuum drying: take out the phase of the acetate esters that contains a large amount of Flavonoid substances, it is carried out decompression distillation, concentrated solution, then this concentrate is carried out vacuum drying, obtain solid persimmon leaf flavone class material.
2, a kind of aqueous two-phase extraction according to claim 1 extracts the method for persimmon leaf flavone class material, it is characterized in that: in aqueous two-phase extraction, can also add inorganic salts when adding PEG polymer and ammonium sulfate aqueous two-phase system.
3, a kind of aqueous two-phase extraction according to claim 1 and 2 extracts the method for persimmon leaf flavone class material, and it is characterized in that: the PEG polymer of adding is 5%～25%, and ammonium sulfate is 10%～20%.
4, according to the method for claim 1 or 2 or 3 described a kind of aqueous two-phase extractions extraction persimmon leaf flavone class materials, it is characterized in that: the molecular weight of the PEG polymer of adding is 300～1500.
5, a kind of aqueous two-phase extraction according to claim 1 and 2 extracts the method for persimmon leaf flavone class material, and it is characterized in that: the inorganic salts of adding can be NaCl or Na
2SO
4
6, a kind of aqueous two-phase extraction according to claim 1 extracts the method for persimmon leaf flavone class material, and it is characterized in that: the acetate esters of adding can be butyl acetate or ethyl acetate.
7, a kind of aqueous two-phase extraction according to claim 1 extracts the method for persimmon leaf flavone class material, it is characterized in that: in aqueous two-phase extraction, and 15 ℃～30 ℃ of phase separation temperature, the time is 2～6 hours.
8, according to the method for claim 1 or 6 described a kind of aqueous two-phase extractions extraction persimmon leaf flavone class materials, it is characterized in that: in the acetate esters back extraction, phase separation temperature is a room temperature, and the time is 1～3 hour.
9, a kind of aqueous two-phase extraction according to claim 1 extracts the method for persimmon leaf flavone class material, and it is characterized in that: in decompression distillation, vacuum drying, the vacuum drying temperature is under 60 ℃～80 ℃.
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|---|---|---|---|
| CNB2004100262405A CN100560173C (en) | 2004-06-17 | 2004-06-17 | A kind of aqueous two-phase extraction extracts the method for persimmon leaf flavone class material |
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|---|---|---|---|
| CNB2004100262405A CN100560173C (en) | 2004-06-17 | 2004-06-17 | A kind of aqueous two-phase extraction extracts the method for persimmon leaf flavone class material |
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| Publication Number | Publication Date |
|---|---|
| CN1709542A true CN1709542A (en) | 2005-12-21 |
| CN100560173C CN100560173C (en) | 2009-11-18 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100519428C (en) * | 2007-10-16 | 2009-07-29 | 中国科学院长春应用化学研究所 | Method for extracting and enriching aromatic compounds in water by double water-phase |
| CN101531652B (en) * | 2009-04-17 | 2012-05-16 | 大连理工大学 | Novel method for extracting anthocyanin in bilberry by double water phases |
| CN102911030A (en) * | 2011-08-02 | 2013-02-06 | 苏州宝泽堂医药科技有限公司 | Aqueous two-phase extraction method of angelica keiskei chalcone |
| CN107188772A (en) * | 2017-05-27 | 2017-09-22 | 浙江工业大学 | A kind of carbamide derivative double-aqueous phase system and its application |
| CN111991440A (en) * | 2020-08-24 | 2020-11-27 | 常州工学院 | Method for extracting flavonoid compounds in cinnamomum camphora by polymer aqueous two-phase extraction |
-
2004
- 2004-06-17 CN CNB2004100262405A patent/CN100560173C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100519428C (en) * | 2007-10-16 | 2009-07-29 | 中国科学院长春应用化学研究所 | Method for extracting and enriching aromatic compounds in water by double water-phase |
| CN101531652B (en) * | 2009-04-17 | 2012-05-16 | 大连理工大学 | Novel method for extracting anthocyanin in bilberry by double water phases |
| CN102911030A (en) * | 2011-08-02 | 2013-02-06 | 苏州宝泽堂医药科技有限公司 | Aqueous two-phase extraction method of angelica keiskei chalcone |
| CN107188772A (en) * | 2017-05-27 | 2017-09-22 | 浙江工业大学 | A kind of carbamide derivative double-aqueous phase system and its application |
| CN107188772B (en) * | 2017-05-27 | 2021-04-06 | 浙江工业大学 | Urea derivative aqueous two-phase system and application thereof |
| CN111991440A (en) * | 2020-08-24 | 2020-11-27 | 常州工学院 | Method for extracting flavonoid compounds in cinnamomum camphora by polymer aqueous two-phase extraction |
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| CN100560173C (en) | 2009-11-18 |
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Granted publication date: 20091118 Termination date: 20120617 |