CN106336390A - Method for extracting flavone from banana leaves - Google Patents
Method for extracting flavone from banana leaves Download PDFInfo
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- CN106336390A CN106336390A CN201610726656.0A CN201610726656A CN106336390A CN 106336390 A CN106336390 A CN 106336390A CN 201610726656 A CN201610726656 A CN 201610726656A CN 106336390 A CN106336390 A CN 106336390A
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- banana leaf
- flavone
- banana
- extracting
- extraction
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
- C07D311/30—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
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- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention belongs to the technical field of extraction of banana leaf active ingredients and particularly provides a method for extracting a flavone compound of banana leaves. According to the extracting process, banana leaves are washed clean, dried, smashed and screened, then banana leaf powder is subjected to extraction and degreasing with petroleum ether, filter residues are collected, a mixture of ethyl alcohol and ethyl acetate serves as an extractant for extraction, filter liquid is taken after filtration and concentrated under a water bath condition, impurities are removed after sufficient settling, filter liquid is collected, and coarse extract liquid is obtained; separation and purification are carried out with polyamide column chromatography, further secondary purification is carried out through crystallization and recrystallization, and purified flavone extract is obtained. The method for extracting flavone of banana leaves is easy to implement, and banana leaves obtained after fruit picking are fully used for extracting flavone; compared with macroporous resin purification, flavone extracted with the method of combining polyamide column chromatography and recrystallization is higher in purity; besides, no special instrument is needed in the extracting process, cost is low, use is safe, the economic value of banana leaves is improved, and the application field of banana leaves is expanded.
Description
Technical field
The present invention relates to the extracting method of Banana Leaf effective ingredient is and in particular to a kind of extracting method of Banana Leaf flavone.
Background technology
Fructus Musae is the monocotyledon of Musaceae Musa, is famous subtropical fruit, is the world's " four big fruit "
One of, China is third place in the world big Fructus Musae manufacturing country, and about 200,000 hectares of Annual planting area is mainly distributed on Guangdong, Guangxi, good fortune
Build, Hainan, the southern part provinces and regions such as Yunnan.Fructus Musae is delicious, nutritious very popular with it, but, banana production
While also produce 75% stem, leaf by-product, when banana is ripe pluck after, the part such as its remaining banana stem leaves is just abandoned
Without causing certain environmental pollution and the wasting of resources.In fact, Fructus Musae is in addition to sarcocarp, the part such as its stem and leaf also all contains
Have flavone etc. enrich have important be worth active component.At present, about Banana Leaf flavone isoreactivity material extraction with
And the research of constituent aspect not yet has play-by-play.Therefore, extract Fructus Musae leaf flavonoid compound and study Banana Leaf Huang
The effect of ketone has very important significance, study a kind of corresponding technology extract that flavone compound has very much from Banana Leaf must
Will.
Content of the invention
The goal of the invention of the present invention is that Banana Leaf is turned waste into wealth, reduce the environmental pollution that causes of Banana Leaf after fruit picking and
Problem of resource waste, for the problems referred to above, provides a kind of method extracting flavone from Banana Leaf.
A kind of extracting method of Fructus Musae leaf flavonoid compound, including extraction process and purification process, concrete operations are as follows:
Extraction process: after Banana Leaf is cleaned, be dried, size-reduced machine is pulverized, cross 60 mesh sieves, make Banana Leaf powder, by Banana Leaf powder
End adds in apparatus,Soxhlet'ses, with petroleum ether, it is carried out extracting defat, collects filtering residue, be immersed in ethyl acetate and second after cooling
Alcohol is extracted with the mixed organic solvents of volume ratio 1:2, and wherein, the concentration of ethanol is 60%～80%, and extracting solution is with 4 layers
Filtered through gauze, filtrate water-bath under the conditions of 60～80 DEG C concentrates, and filter paper filtering after fully precipitating goes the removal of impurity, collects filtrate and obtains
Crude extract immersion；
Purge process: isolated and purified using polyamide column chromatography, then through recrystallization method secondary purification further, obtain
Purification of flavone extract.
In the present invention, further instruction, in extraction process, Banana Leaf powder is initially charged in filtration paper cylinder, places into rope
Family name's extractor, the size of filtration paper cylinder and extractor sizableness.
In the present invention, further instruction, in extraction process, the Banana Leaf powder of addition and the ratio of petroleum ether are 1:
2～1:5g/ml.
In the present invention, further instruction: in extraction process, extraction skimming processes are carried out at room temperature, extract 2～3
Secondary, each 3h.
In the present invention, further instruction, in extraction process, described organic solvent is ethyl acetate and 60%～80%
The mixture as 1:2 finished by ethanol with volume.Every 10g Banana Leaf powder is extracted with 100ml organic solvent.
In the present invention, further instruction, in extraction process, the solid-liquid ratio being added is 1:7～1:9g/ml.
In the present invention, further instruction, in extraction process, the temperature of extraction is 50～70 DEG C.
In the present invention, further instruction, in extraction process, extraction time is 2h, continuously extracts 2 times.
In the present invention, further instruction, in purge process, described amide column chromatography separating purification step is: will
Crude extract immersion is added to the top of polyamide column so as to slowly flow across polyamide column, then with distillation water elution 20min, then uses
, to effluent and hydrochloric acid-magnesium powder no color reaction, eluent is concentrated to no ethanol flavor and dry for 70% ethanol elution.
In the present invention, further instruction, the step of described recrystallization method is: claim 8 is dried gained flavone
It is dissolved in the ethanol solution of heat, filtrate is cooled down by hot solution sucking filtration while hot, place crystallize, then carry out secondary crystallization.
The present invention has the advantages that compared with prior art
The present invention provides a kind of extracting method of Banana Leaf flavone, and Banana Leaf is turned waste into wealth, and reduces the Fructus Musae after fruit picking
Environmental pollution and problem of resource waste that leaf causes；Because ethyl acetate is different from the polarity of ethanol, thus can dissolve the kind of flavone
Class is different, the present invention during extracting, with both mixture as digestion agent, decrease flavone extraction process damage
Lose；During polyamide separating flavone compound, the high adsorption capacity to aglycon for the aqueous mobile phase, the absorption to glycosides in organic phase flow
Ability is strong, using this characteristic, successively uses distilled water and 70% ethanol elution, more fully can elute chromocor compound,
Decrease flavone purge process loss；The side that polyamide column chromatography and recrystallization method combine is adopted in purge process
Method is so that extract flavone high purity 90.13%, and the purity of Flavonoids by Macroporous Adsorption Resin purification is only 84.2%, and described
The method of Banana Leaf extracting flavonoids is simple to operate, the fast institute of extraction rate；In addition extraction process does not need specific apparatus, low cost
Honest and clean, using safety, improve the economic worth of Banana Leaf, widen its application.
Specific embodiment
The invention provides a kind of method of Banana Leaf extracting flavonoids, for making the purpose of the present invention, technical scheme and effect
Clearer, clear and definite, the present invention is described in more detail below.It should be appreciated that specific embodiment described herein is only
In order to explain the present invention, it is not intended to limit the present invention.
Embodiment 1
The method of the Banana Leaf extracting flavonoids that the present invention provides is as follows:
The extraction of Banana Leaf flavone: after Banana Leaf is cleaned, be dried, size-reduced machine is pulverized, cross 60 mesh sieves, make Banana Leaf
Powder, takes 10g Banana Leaf powder to add in apparatus,Soxhlet'ses, with petroleum ether, it is carried out extracting defat, wherein, the Fructus Musae of addition
The ratio of leaf powder and petroleum ether is 1:2g/ml, extracts 3h, repeats extraction step 2 times after collecting filtering residue, collects filter after cooling
Slag, adds the digestion agent that solid-liquid ratio is 1:7g/ml water-bath extraction 2h under the conditions of 50 DEG C to it, wherein, digestion agent is acetic acid second
Ester and 60% ethanol finish the mixture 100ml as 1:3 with volume, collect filtering residue and repeat to extract 1 time, merge lixiviating solution, treat that it is cold
, after temperature-sensitive degree in one's hands, extracting solution is concentrated with 4 layers of filtered through gauze, filtrate water-bath under the conditions of 60 DEG C, filter paper mistake after fully precipitating
Filter, goes the removal of impurity, collects filtrate and obtains crude extract immersion；
The purification of Banana Leaf flavone: take the amount of crude extract immersion half to be added to the top of polyamide column so as to slowly flow across
Polyamide column, then with distillation water elution 20min more anti-with hydrochloric acid-magnesium powder no color with 70% ethanol elution to effluent
Till answering, eluent is concentrated to no ethanol flavor and dry；It is dried in the ethanol solution that gained flavone is dissolved in heat, by thermosol
Liquid sucking filtration while hot, filtrate is cooled down, and places crystallize, then carries out secondary crystallization, that is, obtains flavone extract.
Extraction ratio using spectrophotometry Banana Leaf flavone is 4.213%, and purity is 90.13%.
Purification with macroreticular resin: the ethanol using 95% soaks 1h to ab-8 type macroporous adsorbent resin, makes resin particle
Fully after expansion, it is poured off upper strata ethanol, continue continuously to be washed repeatedly with 95% ethanol, occur without white up to effluent muddy
Till turbid, then it is washed to no ethanol flavor with distillation.The good macroporous adsorbent resin of pretreatment and crude extract immersion are added in container,
The ratio of wherein macroporous adsorbent resin and crude extract immersion is 1:15g/ml, shakes at room temperature, is sufficiently stirred for rear standing adsorption
Overnight, pour out eluent, then with 70% ethanol solution, eluting 20h is carried out to macroporous adsorbent resin, filtrate is collected by filtration, enters
Row concentrate drying, obtains Banana Leaf flavone dry.
Extraction ratio using spectrophotometry Banana Leaf flavone is 4.41%, and purity is 83.3%.
Embodiment 2
The method of the Banana Leaf extracting flavonoids that the present invention provides is as follows:
The extraction of Banana Leaf flavone: after Banana Leaf is cleaned, be dried, size-reduced machine is pulverized, cross 60 mesh sieves, make Banana Leaf
Powder, takes 10g Banana Leaf powder to add in apparatus,Soxhlet'ses, with petroleum ether, it is carried out extracting defat, wherein, the Fructus Musae of addition
The ratio of leaf powder and petroleum ether is 1:4g/ml, extracts 3h, repeats extraction step 2 times after collecting filtering residue, collects filter after cooling
Slag, to its add solid-liquid ratio be 1:8g/ml digestion agent extract 2h under 60 DEG C of parts, wherein, digestion agent be ethyl acetate and
70% ethanol finishes the mixture 100ml as 1:3 with volume, collects filtering residue and repeats to extract 1 time, merges lixiviating solution, treat that it is cooled to
After feel temperature, extracting solution is existed with 4 layers of filtered through gauze, filtrate, and water-bath under the conditions of 70 DEG C concentrates, filter paper filtering after fully precipitating,
Go the removal of impurity, collect filtrate and obtain crude extract immersion；
The purification of Banana Leaf flavone: take the amount of crude extract immersion half to be added to the top of polyamide column so as to slowly flow across
Polyamide column, then with distillation water elution 20min, then with 70% ethanol elution to effluent and hydrochloric acid-magnesium powder no color reaction
Till, eluent is concentrated to no ethanol flavor and dry；It is dried in the ethanol solution that gained flavone is dissolved in heat, by hot solution
Sucking filtration while hot, filtrate is cooled down, and places crystallize, then carries out secondary crystallization, that is, obtains flavone extract.
Extraction ratio using spectrophotometry Banana Leaf flavone is 4.83%, and purity is 90.05%.
Macroporous adsorbent resin purification: the ethanol using 95% soaks 1h to ab-8 type macroporous adsorbent resin, makes resin particle fill
Divide after expanding, be poured off upper strata ethanol, the continuous washing of ethanol continuing with 95% is multiple, until effluent occurs without white opacity
Till, then it is washed to no ethanol flavor with distillation.The good macroporous adsorbent resin of pretreatment and crude extract immersion are added in container, its
The ratio of middle macroporous adsorbent resin and crude extract immersion is 1:20g/ml, shakes at room temperature, is sufficiently stirred for rear standing adsorption mistake
At night, pour out eluent, then with 70% ethanol solution, eluting 20h is carried out to macroporous adsorbent resin, filtrate is collected by filtration, carries out
Concentrate drying, obtains Banana Leaf flavone dry.
Extraction ratio using spectrophotometry Banana Leaf flavone is 4.72%, and purity is 84.05%.
Embodiment 3
The method of the Banana Leaf extracting flavonoids that the present invention provides is as follows:
The extraction of Banana Leaf flavone: after Banana Leaf is cleaned, be dried, size-reduced machine is pulverized, cross 60 mesh sieves, make Banana Leaf
Powder, takes 10g Banana Leaf powder to add in apparatus,Soxhlet'ses, with petroleum ether, it is carried out extracting defat, wherein, the Fructus Musae of addition
The ratio of leaf powder and petroleum ether is 1:5g/ml, extracts 3h, repeats extraction step 2 times after collecting filtering residue, collects filter after cooling
Slag, to its add solid-liquid ratio be 1:9g/ml digestion agent extract 2h under 70 DEG C of parts, wherein, digestion agent be ethyl acetate and
80% ethanol finishes the mixture 100ml as 1:3 with volume, collects filtering residue and repeats to extract 1 time, merges lixiviating solution, treat that it is cooled to
After feel temperature, extracting solution is existed with 4 layers of filtered through gauze, filtrate, and water-bath under the conditions of 80 DEG C concentrates, filter paper filtering after fully precipitating,
Go the removal of impurity, collect filtrate and obtain crude extract immersion；
The purification of Banana Leaf flavone: take the amount of crude extract immersion half to be added to the top of polyamide column so as to slowly flow across
Polyamide column, then with distillation water elution 20min, then with 70% ethanol elution to effluent and hydrochloric acid-magnesium powder no color reaction
Till, eluent is concentrated to no ethanol flavor and dry；It is dried in the ethanol solution that gained flavone is dissolved in heat, by hot solution
Sucking filtration while hot, filtrate is cooled down, and places crystallize, then carries out secondary crystallization, that is, obtains flavone extract.
Extraction ratio using spectrophotometry Banana Leaf flavone is 4.67%, and purity is 89.79%.
Purification with macroreticular resin: the ethanol using 95% soaks 1h to ab-8 type macroporous adsorbent resin, makes resin particle
Fully after expansion, it is poured off upper strata ethanol, continue continuously to be washed repeatedly with 95% ethanol, occur without white up to effluent muddy
Till turbid, then it is washed to no ethanol flavor with distillation.The good macroporous adsorbent resin of pretreatment and crude extract immersion man are added container
In, the ratio of wherein macroporous adsorbent resin and crude extract immersion is 1:25g/ml, shakes at room temperature, and after being sufficiently stirred for, standing is inhaled
Attached overnight pour out eluent, then with 70% ethanol solution, eluting 20h carried out to macroporous adsorbent resin, filtrate is collected by filtration,
Carry out concentrate drying, obtain Banana Leaf flavone dry.
Extraction ratio using spectrophotometry Banana Leaf flavone is 4.59%, and purity is 84.2%.
Described above is the detailed description for the preferable possible embodiments of the present invention, but embodiment is not limited to this
Bright patent claim, the equal change being completed under the technical spirit suggested by all present invention or modification change, all should belong to
In the covered the scope of the claims of the present invention.
Claims (10)
1. a kind of extracting method of Fructus Musae leaf flavonoid compound is it is characterised in that include extraction process and purification process, specifically
Operation is as follows:
A. extraction process: after Banana Leaf is cleaned, it is dried, size-reduced machine is pulverized, cross 40～80 mesh sieves, make Banana Leaf powder,
Weigh Banana Leaf powder to add in apparatus,Soxhlet'ses, with petroleum ether, it is carried out extracting defat, collect filtering residue after cooling, be immersed in
Extracted in organic solvent, with 4 layers of filtered through gauze, by the filtrate obtaining, under the conditions of 60～80 DEG C, water-bath concentrates extracting solution,
Using filter paper filtering after fully precipitating, go the removal of impurity, collect filtrate and obtain crude extract immersion；
B. purification process: isolated and purified using polyamide column chromatography, then through recrystallization method secondary purification further, obtain pure
Change flavone extract.
2. Banana Leaf flavone according to claim 1 extracting method it is characterised in that: in extraction process, Banana Leaf powder
End is initially charged in filtration paper cylinder, places into apparatus,Soxhlet'ses, and filtration paper cylinder is close to extractor inwall.
3. Banana Leaf flavone according to claim 1 extracting method it is characterised in that: in extraction process, the perfume (or spice) of addition
The ratio of any of several broadleaf plants leaf powder and petroleum ether is 1:2～1:5g/ml.
4. Banana Leaf flavone according to claim 1 extracting method it is characterised in that: in extraction process, extract defat
Process is carried out at room temperature, extracts 2～3 times, each 3h.
5. Banana Leaf flavone according to claim 1 extracting method it is characterised in that: in extraction process, described organic
Solvent is ethyl acetate and the mixture with volume ratio as 1:3 for 60%～80% ethanol.Every 10g Banana Leaf powder is had with 100ml
Machine extraction.
6. Banana Leaf flavone according to claim 1 extracting method it is characterised in that: in extraction process, added
Solid-liquid ratio is 1:7～1:9g/ml.
7. Banana Leaf flavone according to claim 1 extracting method it is characterised in that: in extraction process, the temperature of extraction
Spend for 50～70 DEG C.
8. Banana Leaf flavone according to claim 1 extracting method it is characterised in that: in extraction process, extraction time
For 2h, continuously extract 2 times.
9. the extracting method of Banana Leaf flavone according to claim 1 is it is characterised in that described polyamide column chromatography divides
From purification step it is: crude extract immersion is added to the top of polyamide column so as to slowly flow across polyamide column, then uses distilled water
Eluting 20min, then with 70% ethanol elution to effluent and hydrochloric acid-magnesium powder no color reaction, eluent concentrated to no
Ethanol flavor, and be dried.
10. the extracting method of Banana Leaf flavone according to claim 1 is it is characterised in that the step of described recrystallization method
For: claim 8 is dried in the ethanol solution that gained flavone is dissolved in heat, filtrate is cooled down, puts by hot solution sucking filtration while hot
Put crystallize, then carry out secondary crystallization.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610726656.0A CN106336390A (en) | 2016-08-25 | 2016-08-25 | Method for extracting flavone from banana leaves |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610726656.0A CN106336390A (en) | 2016-08-25 | 2016-08-25 | Method for extracting flavone from banana leaves |
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| CN106336390A true CN106336390A (en) | 2017-01-18 |
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ID=57824942
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610726656.0A Pending CN106336390A (en) | 2016-08-25 | 2016-08-25 | Method for extracting flavone from banana leaves |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110123921A (en) * | 2019-06-03 | 2019-08-16 | 广西中医药大学 | The preparation method and anti-dengue virus application of banana leaf extract |
| CN111544923A (en) * | 2020-05-08 | 2020-08-18 | 河北瑞龙生物科技有限公司 | Preparation method of snow pear extract for cigarettes |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102697988A (en) * | 2012-06-04 | 2012-10-03 | 杨公明 | Method for extracting flavone from banana skin |
-
2016
- 2016-08-25 CN CN201610726656.0A patent/CN106336390A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102697988A (en) * | 2012-06-04 | 2012-10-03 | 杨公明 | Method for extracting flavone from banana skin |
Non-Patent Citations (4)
| Title |
|---|
| 周银丽等: "芭蕉花中总黄酮的最佳提取工艺", 《江苏农业科学》 * |
| 李子健: "香蕉副产物的开发利用研究", 《中国优秀硕士学位论文全文数据库（硕士） 农业科技辑》 * |
| 王妙飞等: "香蕉皮中总黄酮的提取工艺", 《光谱实验室》 * |
| 顾采琴等: "香蕉皮黄酮的分离纯化及抑茵活性研究", 《食品科学》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110123921A (en) * | 2019-06-03 | 2019-08-16 | 广西中医药大学 | The preparation method and anti-dengue virus application of banana leaf extract |
| CN110123921B (en) * | 2019-06-03 | 2022-03-01 | 广西中医药大学 | Preparation method of banana leaf extract and application of banana leaf extract in resisting dengue fever virus |
| CN111544923A (en) * | 2020-05-08 | 2020-08-18 | 河北瑞龙生物科技有限公司 | Preparation method of snow pear extract for cigarettes |
| CN111544923B (en) * | 2020-05-08 | 2021-12-10 | 河北瑞龙生物科技有限公司 | Preparation method of snow pear extract for cigarettes |
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