CN1813823A - Method for extracting flavone from pine needle - Google Patents
Method for extracting flavone from pine needle Download PDFInfo
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- CN1813823A CN1813823A CN 200510005386 CN200510005386A CN1813823A CN 1813823 A CN1813823 A CN 1813823A CN 200510005386 CN200510005386 CN 200510005386 CN 200510005386 A CN200510005386 A CN 200510005386A CN 1813823 A CN1813823 A CN 1813823A
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- folium pini
- flavone
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Abstract
The present invention relates to a method for extracting flavone from natural pine needle. Said method includes the following steps: cutting cleaned pine needle, using 30-90 wt% of ethyl alcohol aqueous solution as extraction solution, material-liquid ratio (weight ratio) is 1:10-50, heating for 1-5 hr at 20-100 deg.C, reduced pressure filtration and concentrating filtrate so as to obtain the flavone extract.
Description
Technical field
The invention belongs to the Chinese medicine extraction field, specifically relate to a kind of method of from natural pine needle, extracting flavone.
Background technology
Whole world confierophyte most species, wherein only pinaster just has kind more than 100, is one of the widest seeds of Northern Hemisphere distribution.Folium Pini (Pineneedles) as its main by-product is the leaf of Pinaceae (Pinaceae) Pinus (Pinus) plant, another name bristles Folium Pini, Folium Pini, illawarra mountain pine palpus.China has abundant Folium Pini resource.The pinaster of China is various in style, distributes not only extensively but also relatively concentrated.In China south abundant Pinus massoniana Lamb, pinus elliottii, pinus yunnanensis faranch, Pinus taiwanesis etc. are arranged; And there are Pinus koraiensis, Pollen pini thunbergii, Cedrus deoclar (Roxb.) G. Don etc. in the north; In addition, also have large-scale pine forest districts such as big Xi Anling, little Xi Anling, Wuyi Mountain Range, kind surplus in the of totally 30.The existing Folium Pini area of China is about 6100～6,700 ten thousand hm
2, only the reserves of pine needle are just more than 100,000,000 tons.About 70,000 hm of the domestic annual area of the final fell in each main forest zone
2, adding has 2,500 ten thousand hm national every year
2Earsh in the tending and intermittent cutting of forest woods only can obtain about 4,000,000 tons of pine needle this every year, can be processed into about 2,300,000 tons of pine needle powder.(the biology magazine, 1996, (2): 25, forest chemical engineering communication, 2003,37 (4): 29-34, Yunnan University of Traditional Chinese Medicine's journal, 1997,20 (3)) because the Folium Pini reproduction speed is fast, sustainable use, resource is extremely abundant, thereby is a kind of natural resources with huge potentiality to be exploited.
Compendium of Material Medica (Compendium of Materia Medica (volume two), People's Health Publisher, 1982.1917) record: " nontoxic, clothes make us not old for a long time for Folium Pini, abnormal smells from the patient hardship, temperature, and the QI invigorating of making light of one's life by commiting suicide cures mainly rheumatism skin ulcer, killing parasites for relieving itching.Treatment rheumatism flaccidity syndrome and arthralgia syndrome, traumatic injury, insomnia, edema, eczema, scabies, and can prevent epidemic encephalitis, influenza, ancylostomiasis etc." during the contained 120 kinds of first-class medicines of beam is chatted for the TAO Hong-Jing Collective Notes to the Canon of Materia medica and the legendary god of farming selects 365 kinds of medicines, classify strobile and Folium Pini as first-class medicine first.Its Colophonium, Strobilus Pini, Folium Pini successive dynasties all go into medicinal.And the Folium Pini collection is the most convenient, and it is used as medicine the earliest and is documented in (Chinese medicine voluminous dictionary (first volume), the Shanghai People's Press in " Mingyi Bielu ".1977.1254), write in the book: " Folium Pini, bitter in the mouth temperature cure mainly the rheumatism stagnated QI, piliation, and settling five organs, not hungry in keeping, prolong life.”
Medical circle compares systematic research to the pharmacological action of Folium Pini both at home and abroad, result of study shows, the main pharmacological of Folium Pini has three: (1) delaying senility effect: contained VE is a kind of natural grease soluble antioxidant in the extract from pine needles, can dissolve intravital aging thing, adjust and promotion body tissue ability, the peroxidation of prevention and inhibition organism film, the delaying senility effect.Taking drosophila survival laboratory method proof Folium Pini water extract is in the 10%-40% scope, can make the life-span of fruit bat adult prolong (hubei agricultural science, 2003,1) extremely significantly.(2) press down tumor, antimutagenic effect, raise immunity (Chinese medicine research, 1999; (2): 31, new Chinese medicine and clinical pharmacology, 1997,8 (4): 219, Food Science, 1994; (2): 52, Guizhou medicine, 1997); (3) effect for reducing blood fat (Beijing University of Chinese Medicine's journal, 2001,24 (2): 35, Zhejiang College Of Traditional Chinese Medicine journal, 1992,16 (3): 30).Special needs to be pointed out is: according to zoopery, the toxicity of extract from pine needles is extremely low, can be used as a kind of nutrition and dietetic therapy resource of novelty.(Food Science, 1989, (10): 37～38)
The main chemical compositions of Folium Pini has volatile oil, protein, aminoacid, vitamin, chlorophyll etc., and wherein main active substances is a flavone compound.(the northwest Botany Gazette, 1990,10 (3): 232-236) modern pharmacological research shows (Food Additives Used in China, 2003.5), and flavone compound has tangible pharmacological action at cardiovascular system, hormonal system and anti-tumor aspect.Particularly Antioxidative Property of Flavonoid causes scholars' extensive concern, its structure is imitated with the relation of oxidability further investigate, now clear and definite mechanism.
The technology of existing extensive solvent extraction flavone mainly comprises three classes: water extraction, alkaline water or alkaline rare alcohol extraction are followed the example of and the organic solvent extraction method, low, the safety of water extraction technology cost, be fit to industrialized great production, but when using water extraction, impurity more (as inorganic salt, protein, sugar etc.) in the extracting solution, further separation costs increases, and the purity and the quality of product are lower.Flavonoid substances has phenolic hydroxyl group mostly, therefore can be with alkaline water or alkaline rare alcohol extraction, and extraction ratio increases than water extraction, but is complicated component in the extracting solution equally, and flavones content is not high.The organic solvent extraction method is simple to equipment requirements, product yield height.But cost is higher, and time-consuming length is unfavorable for the market competition of product.Desolventize outside the extraction method, also have microwave method, supercritical ultrasonics technology and macroreticular resin absorbing method etc. at present, though these methods have its unique distinction, it is former thereby temporarily be not extensive use of that because its scope of application is limited, equipment cost is higher, complex process, technology are still immature etc.
Summary of the invention
The objective of the invention is to overcome prior art water extraction, alkaline water or alkaline rare alcohol extraction, to follow the example of in the extract impurity more, organic solvent extraction method cost is higher, the defective of time-consuming length, thereby a kind of extraction ratio height is provided, and the method for from Folium Pini, extracting flavone simple, with low cost.
The objective of the invention is to realize by the following technical solutions:
The method of extracting flavone from Folium Pini provided by the invention comprises following step:
With the Folium Pini chopping of cleaning (for example being broken to 2～3cm/ segment), the ethanol water that uses 30～90wt% then is as extracting solution, solid-liquid ratio (weight ratio) is 1: 10～50, extracted in 1～5 hour 20～100 ℃ of heating, carry out filtration under diminished pressure while hot, obtain flavone extract after filtrate is concentrated.
In order to improve extraction efficiency, this method is carried out pretreatment to the raw material Folium Pini before also being included in and extracting, for example dry or pulverizing.
Do reference material with rutin and make standard curve, measure content of total flavone in the extract with ultra-violet absorption spectrum.
The mixed solvent that the method for extracting flavone from Folium Pini provided by the invention is used ethanol/water extracts the natural product Folium Pini under heating-up temperature, can obtain flavone in high yield ground.This method is to carry out according to the similar principle that mixes.Its process nature is the mass transport process that flavone compound shifts to solvent from inside plants: at first, solvent molecule is delivered to the surface of Folium Pini solid particle from the solvent main body; Secondly, the solvent molecule diffusion is infiltrated in Folium Pini solid interior and its inner micropore; Then, the dissolving of the flavone compound in the Folium Pini enters solvent; Next, by the surface of the solution diffusion in the passage of Folium Pini solid micropore to Folium Pini; At last, flavone compound is delivered to the solvent main body from the Folium Pini surface of solids.Wherein, flavone compound dissolubility size and be two principal elements that influence extraction ratio in selected solvent (extracting solution) to the complexity of solvent diffuse.And the diffusion velocity of flavone compound in selected solvent depends on the factors of extracting between temperature, solution viscosity, diffusion area and the two-phase interface such as concentration difference.
Flavone compound is present in the plant cell usually, and the diffusional resistance that cell membrane produces makes that its lixiviate speed ratio is less.Carry out such as drying or the pretreatment pulverizing to raw material, help breaking of plant cell membrane, solvent also enters the inner directly dissolving of plant cell flavonoid easily, thereby can improve extraction efficiency.
The advantage that extracts the method for flavone from Folium Pini provided by the invention is:
1, simple: should method is simple, the gentle and control easily of experiment condition;
2, efficient: flavones content is higher in the extracting solution, and promptly yield is higher;
3, with low cost: owing to there is not adding other organic solvent except that ethanol in the course of reaction, therefore can not introduce other impurity in leaching process, this has just simplified the step of separation and purification greatly, has reduced the cost of separation and purification;
4, environmental protection: the solvent that is used to extract can recycle, so leaching process does not have waste liquid to get rid of, helps environmental conservation.
Description of drawings
Fig. 1 is the rutoside standard sample uv atlas of the embodiment of the invention 1; Represent the absorbance standard curve of 0.01g rutin/ml (30% ethanol), 0.02g rutin/ml (30% ethanol), 0.04g rutin/ml (30% ethanol), 0.06g rutin/ml (30% ethanol), 0.08g rutin/ml (30% ethanol), 0.10g rutin/ml (30% ethanol), 0.12g rutin/ml (30% ethanol) from the bottom to top respectively.
Fig. 2 be the alcohol extraction sample uv atlas (descending) of the embodiment of the invention 1 with the uv atlas of 0.06g rutin/ml (30% ethanol) (on).
The specific embodiment
Embodiment 1,
With the Folium Pini chopping of cleaning, the ethanol water that uses 40wt% then is as extracting solution, and solid-liquid ratio (weight ratio) is 1: 15, extracts in 1 hour 25 ℃ of heating, carries out filtration under diminished pressure while hot, obtains flavone extract after filtrate is concentrated.
According to langbobier law, the concentration and the absorbance of flavone are linear dependence, determine the flavones content in the extracting solution.Be reference material with the rutin that contains flavone at first, make the standard curve of ultra-violet absorption spectrum, concrete grammar is: the rutin sample is dried to constant weight in 200 ℃ of baking ovens, accurately take by weighing 0.0200g, the ethanol standardize solution with 30% is in the 100mL volumetric flask.Get 1,2,4,6,8,10 respectively, 12ml in the volumetric flask of 50mL, the ethanol standardize solution with 30%.Respectively get 5mL in the volumetric flask of 25mL, add 0.7mL0.5%NaNO
2, add 0.7mL10%Al (NO
3)
3, shake up, add the NaOH of 5mL4% behind the placement 5min, shake up ethanol standardize solution with 30%.Survey uv atlas behind the 10min, the absorbance at record 500nm place is done linear regression with method of least square, gets the standard curve of rutin concentration and absorbance, as shown in Figure 1.
Then, measure content of total flavone in the said extracted thing with ultra-violet absorption spectrum: get 1mL said extracted liquid in the 50mL volumetric flask with 30% ethanol standardize solution; Get the 5mL diluent in the 25mL volumetric flask, add 0.7mL0.5%NaNO
2, add 0.7mL10%Al (NO
3)
3, shake up, add the NaOH of 5mL4% behind the placement 5min, shake up ethanol standardize solution with 30%; Survey ultra-violet absorption spectrum behind the 10min, as shown in Figure 2, the absorbance at record 345nm, 356nm, 500nm place according to standard curve as can be known, contains 4.78% flavone in this extracting solution.
Embodiment 2,
With the Folium Pini chopping of cleaning, the ethanol water that uses 30wt% then is as extracting solution, and solid-liquid ratio (weight ratio) is 1: 15, extracts in 1 hour 35 ℃ of heating, carries out filtration under diminished pressure while hot, obtains flavone extract after filtrate is concentrated.
Use the method among the embodiment 1, measure and contain 4.51% (quality percentage composition) flavone down together in this extracting solution.
Embodiment 3,
With the Folium Pini chopping of cleaning, the ethanol water that uses 30wt% then is as extracting solution, and solid-liquid ratio (weight ratio) is 1: 25, extracts in 1 hour 35 ℃ of heating, carries out filtration under diminished pressure while hot, obtains flavone extract after filtrate is concentrated.
Use the method among the embodiment 1, measure and contain 4.66% flavone in this extracting solution.
Embodiment 4,
With the Folium Pini chopping of cleaning, the ethanol water that uses 60wt% then is as extracting solution, and solid-liquid ratio (weight ratio) is 1: 15, extracts in 1 hour 40 ℃ of heating, carries out filtration under diminished pressure while hot, obtains flavone extract after filtrate is concentrated.
Use the method among the embodiment 1, measure and contain 5.32% flavone in this extracting solution.
Embodiment 5,
With the Folium Pini chopping of cleaning, the ethanol water that uses 90wt% then is as extracting solution, and solid-liquid ratio (weight ratio) is 1: 10, extracts in 5 hours 20 ℃ of heating, carries out filtration under diminished pressure while hot, obtains flavone extract after filtrate is concentrated.
Use the method among the embodiment 1, measure and contain 5.41% flavone in this extracting solution.
Embodiment 6,
With the Folium Pini chopping of cleaning, the ethanol water that uses 30wt% then is as extracting solution, and solid-liquid ratio (weight ratio) is 1: 50, extracts in 3 hours 100 ℃ of heating, carries out filtration under diminished pressure while hot, obtains flavone extract after filtrate is concentrated.
Use the method among the embodiment 1, measure and contain 5.49% flavone in this extracting solution.
Claims (4)
1, a kind of method of from Folium Pini, extracting flavone, comprise following step: with the Folium Pini chopping of cleaning, the ethanol water that uses 30～90wt% then is as extracting solution, the weight ratio of feed liquid is 1: 10～50, extracted in 1～5 hour 20～100 ℃ of heating, carry out filtration under diminished pressure while hot, obtain flavone extract after filtrate is concentrated.
2, the method for extracting flavone from Folium Pini as claimed in claim 1 is characterized in that: this method is carried out pretreatment to the raw material Folium Pini before also being included in and extracting.
3, the method for extracting flavone from Folium Pini as claimed in claim 1, it is characterized in that: described pretreatment is for to carry out drying to Folium Pini.
4, the method for extracting flavone from Folium Pini as claimed in claim 1, it is characterized in that: described pretreatment is for to pulverize Folium Pini.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200510005386 CN1813823A (en) | 2005-02-05 | 2005-02-05 | Method for extracting flavone from pine needle |
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| CN 200510005386 CN1813823A (en) | 2005-02-05 | 2005-02-05 | Method for extracting flavone from pine needle |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101549013B (en) * | 2009-05-13 | 2012-10-03 | 文永盛 | Capsule, tablet and granules of minium and preparation method |
| CN103505479A (en) * | 2013-09-12 | 2014-01-15 | 中国计量学院 | Preparation method of pine needle flavone |
| CN103828911A (en) * | 2012-11-21 | 2014-06-04 | 金华职业技术学院 | Fresh-keeping method of bergamot fruits with pine needle extract |
| CN108077829A (en) * | 2018-01-10 | 2018-05-29 | 山东青果食品有限公司 | A kind of processing method based on reduction vegetables nutrient loss |
-
2005
- 2005-02-05 CN CN 200510005386 patent/CN1813823A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101549013B (en) * | 2009-05-13 | 2012-10-03 | 文永盛 | Capsule, tablet and granules of minium and preparation method |
| CN103828911A (en) * | 2012-11-21 | 2014-06-04 | 金华职业技术学院 | Fresh-keeping method of bergamot fruits with pine needle extract |
| CN103505479A (en) * | 2013-09-12 | 2014-01-15 | 中国计量学院 | Preparation method of pine needle flavone |
| CN103505479B (en) * | 2013-09-12 | 2015-03-25 | 中国计量学院 | Preparation method of pine needle flavone |
| CN108077829A (en) * | 2018-01-10 | 2018-05-29 | 山东青果食品有限公司 | A kind of processing method based on reduction vegetables nutrient loss |
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