CN102040579A - Method for extracting luteolin from peanut roots, stems, leaves and shells - Google Patents

Method for extracting luteolin from peanut roots, stems, leaves and shells Download PDF

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CN102040579A
CN102040579A CN2011100264699A CN201110026469A CN102040579A CN 102040579 A CN102040579 A CN 102040579A CN 2011100264699 A CN2011100264699 A CN 2011100264699A CN 201110026469 A CN201110026469 A CN 201110026469A CN 102040579 A CN102040579 A CN 102040579A
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luteolin
ethanol
peanut
crystallization
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彭国平
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彭国平
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Abstract

The invention relates to a method for extracting luteolin from peanut roots, stems, leaves and shells, comprising the following steps: washing materials comprising peanut roots, stems, leaves and shells, removing impurities in the peanut roots, stems, leaves and shells, and grinding the peanut roots, stems, leaves and shells subject to impurity removal; extracting by using 75% ethanol, filtering, decoloring, and concentrating at reduced pressure; precipitating by using hot water, filtering, heating filtrate, and concentrating at reduced pressure; absorbing by using KLFC-150 macroporous resin, and eluting by using 75% ethanol; concentrating elution solution at reduced pressureto obtain crude luteolin; dissolving the crude luteolin in ethanol, adding water to dilute the crude luteolin, recovering the ethanol, concentrating, crystallizing, and recrystallizing to obtain the high-purity luteolin product. The operation process is mainly characterized in that the peanut roots, stems, leaves and shells are used as extraction raw materials and are low-cost sustainable resources, the 75% ethanol is used as extraction solvent and eluent, and the product contains no toxic solvent and other residue, is safe and environmentally friendly and is low in production cost and high in yield.

Description

A kind of method of utilizing peanut root, stem, leaf, shell to extract luteolin
Technical field
The present invention relates to a kind of method of utilizing peanut root, stem, leaf, shell to extract luteolin, belong to the technical field of natural product chemistry.
Background technology
Luteolin (Luteolin), be the effective constituent of from the Herba Ajugae (Ajugadecumbens Thunb) that produce in the herbal medicine Herba Dracocephali Integrifolii (Dracocephalumintegrifolium Bge.) and the Anhui of Xinjiang treatment trachitis, separating at first, it is a kind of slightly acidic kaempferol compounds, widely distributed at occurring in nature, can from multiple natural medicinal plant, vegetables, fruit, separate obtaining.The chemical analysis of standard program studies show that, compares with Quercetin and capsaicine etc. the luteolin under the volumetric molar concentration condition, and luteolin has the strongest anti-oxidant activity, and its oxidation-resistance can be used to suppress the Kazakhstan of oleaginous food and loses.The result of pharmacology and clinical experiment shows that luteolin has the effect of antibiotic, antiviral, blood fat reducing and cholesterol, preventing cardiovascular disease in vivo; In recent years, a large amount of domestic and foreign literatures has been reported the anti-tumor activity of luteolin, and the result shows that it has remarkable restraining effect to kinds of tumors, can disturb tumour cell metabolism, cell growth inhibiting, cell death inducing.It is a kind of legal food color that luteolin is also abroad confirmed as.
The pure product of luteolin are a kind of golden yellow powder, and are normally isolated for containing the golden yellow needle crystal of a water molecules from ethanol.Can be dissolved in organic solvents such as ethanol, ether; Be slightly soluble in hot water, be insoluble in cold water.It is pleasing faint yellow that the aqueous solution is, and is dissolved in 10% aqueous sodium hydroxide solution, and is deep yellow, is dissolved in the vitriol oil and generates zinc salt, is dark red yellow.Because of existing phenolic hydroxyl group,, can generate colored complex compound on the luteolin molecule with metal ions such as iron, magnesium, calcium, copper, aluminium, zirconiums so its aqueous solution shows faint acidity.
Peanut is second largest food plant oil sources of China and protein resource, and its waste products Pericarppium arachidis hypogaeae has been used as the extraction raw material of luteolin, obtains comprehensive utilization.But peanut root, stem, leaf are except seldom partly being used to feed processing, and wherein a large amount of peanut stem leafs is taken as waste or fuel, causes the significant wastage of resource, and resource utilization is very low, has directly influenced the comprehensive utilization value and the economic benefit of peanut.
Publication number is the method that the Chinese patent of CN1666987 has been introduced a kind of synthetic luteolin newly; this method is starting raw material with the Phloroglucinol; need not protecting group; directly with 3; the condensation of 4-dimethoxy benzoyl acetic acid ethyl ester, cyclization get 3 ', 4 '-dimethoxy-5, the 7-dihydroxyflavone; get luteolin, total recovery 34.2% through aluminum chloride/pyridine catalysis demethylation then.
Publication number is that to have introduced a kind of be the method for the synthetic luteolin of basic raw material with the natural extract to the Chinese patent of CN1544427.The technology that existing total synthesis method prepares luteolin is extremely complicated, and production cost is higher.The present invention is raw material with the Hesperidin, and synthetic method comprises that a. synthesizes diosmin; B. synthetic diosmetin; C. synthetic three steps of luteolin, the whole synthesis technique raw material of the present invention cheaply is easy to get, and is simple to operate, stable reaction conditions, control easily, product is easy to separation and purification, and total yield of products can reach 40~47%, purity reaches 95%, and production cost is lower, and environmental pollution is little.
Publication number is the preparation method that the Chinese patent of CN1687054 has been introduced a kind of compound of luteolin.Its step comprises: prior to adding raw material rutin or derivatives thereof in the water, add NaOH and dissolve fully to raw material under heating and agitation condition, be cooled to room temperature, regulate pH=2~6, filter, washing, the dry raw material elaboration that gets; In water, add solid alkali then, add the raw material elaboration and the Na2S2O4 that make, consumption in molar ratio, raw material elaboration: solid alkali: Na2S2O4: water is 1: 15~20: 8~70: 1110~3330,100~500W microwave heating refluxed 0.25~2 hour, be cooled to room temperature, conditioned reaction liquid pH=2~7, filtration, washing, drying; Carry out recrystallization with organic solvent again.The present invention is a raw material with the rutin or derivatives thereof, synthetic luteolin, with low cost, the reaction times is short, easy and simple to handle and easy to control, products therefrom purity and yield are higher.
Publication number is that the Chinese patent of CN1974590 has been introduced a kind of method from the plant extract medicine, relate in particular to a kind of method of from East Perillae, extracting luteolin-7-O-β-D-glucoside, East Perillae is utilized solvent extraction, concentrated solution or medicinal extract after extracting is water-soluble, organic extractant extraction degreasing with low-pole or middle polarity, water after the degreasing is used and the immiscible low-carbon alcohol kind of extractants extraction of water again, the extraction phase concentrate drying gets luteolin-7-O-β-D-glucoside behind the recrystallization; Perhaps the water after the degreasing is crossed macroporous adsorbent resin, the eluent wash-out, and the elutriant concentrate drying gets luteolin-7-O-β-D-glucoside behind the recrystallization; Extraction process of the present invention is simple, and is easy to prepare, and energy consumption is little, non-environmental-pollution, and solvent can be recycled, and the extraction yield height can be used for researching and developing the medicine of diseases such as treatment cardiovascular and cerebrovascular diseases, bronchitis, asthma, lung cancer.
Publication number is the method that the Chinese patent of CN1903815 has been introduced resveratrol in a kind of supersound extraction peanut root, may further comprise the steps: (1) is taken root dried flower and is pulverized the back alcohol immersion; (2) will under water-bath, carry out ultrasound-enhanced extraction through the peanut root that step (1) is handled; (3) suction filtration while hot, extracting solution and decompression and solvent recovery, distillation are concentrated into the thick paste shape; (4) with obtaining heavy paste extract water heating for dissolving, add ethyl acetate extraction, transferring its pH value with alkali is 7.0~10.0, leaves standstill, suction filtration, concentrating under reduced pressure get thick paste shape resveratrol crude extract.The inventive method is simple, extracts convenient, fastly, and raw material sources are abundant, and production cost is low, and the content of resveratrol can reach more than 1.0% in the extract.
Application number is that 200810147435.3 Chinese patent has been introduced a kind of method of utilizing the fermentation of Aspergillus niger resveratrol extracted from peanut root, it is characterized in that the cellulase degradation resveratrol extracted from peanut root that utilizes the fermentation of peanut root to produce.The invention has the advantages that the cellulase that utilizes peanut root fermentation of Aspergillus niger to produce replaces the plain enzyme of commercial fibre to carry out Enzymatic Extraction; and utilize Enzymatic Extraction trans-resveratrol extraction time weak point; the extraction conditions gentleness; improved the trans-resveratrol yield greatly; greatly reduce the production cost of trans-resveratrol, be more suitable for extensive chemical industry production.
Publication number is the preparation method that the Chinese patent of CN1515521 has been introduced a kind of peanut leaf extract, it is characterized in that this method is with the peanut stem leaf drying, pulverize, behind 10~40 mesh sieve holes, place the heating of strap clamp cover and backflow is arranged, in the polyfunctional reactant pot of water distilling apparatus, 144 parts of Folium Arachidis hypogaeae are earlier with 200~1000 parts of non-polar solution (ether, sherwood oil) reflux is 1~3 time, each 2~4h, also the used water vapor distillation method extracts fat-soluble component A, residual leaf is used 200~1200 parts of polar solvent (ethanol again, water) refluxing extraction is 1~3 time, 1~4h once more, two kinds of extracting liquid filterings, the extracting solution merging is condensed into medicinal extract, about 10% (the medicinal extract water content about 50%) of yield, get medicinal extract, mix with inert filler, after 70 ℃ of dryings, be ground into fine powder, the apparatus,Soxhlet's of packing into, use sherwood oil in succession, ethyl acetate, acetone, dehydrated alcohol extraction, also can be according to the type of compounds that exists in the Folium Arachidis hypogaeae, the application specific solvent extraction separates, make different generic compound parts, A is for overall: B is that protein: C is that polysaccharide: D is a flavones, tannin: E is a lipoclastic, volatile oil.
Publication number is the production method of peanut stem extract that the Chinese patent of CN1788626 has been introduced a kind of blood sugar regulation, it is characterized in that: wherein earlier peanut stem washing back is dried in normal temperature, or in low temperature heating, drying below 50 ℃, get the water that the dry portion adds 10~300 parts this moment is solvent, make the temperature can be through heating slowly at 50~100 ℃, keep 1~4h extraction, in with peanut stem after the contained complete stripping of composition, filtered, promptly get the extraction liquid that contains special composition, with after this extraction liquid process instantaneous sterilization, utilize automatic filling machine to charge into Aluminium Foil Package automatically at once again, in aluminium pot or the PET bottle, directly drink through after the sterilization again as beverage; Perhaps, further extraction liquid is made paste, it will extract the extraction liquid that contains special composition out in the peanut stem, utilize vacuum or pressure regulating equipment, and carries out thickening to suitable paste at low temperature; Perhaps, further extraction liquid is made powder or powder again, it will extract the extraction liquid that contains special composition out in the peanut stem, made paste is when being evaporated to 1/5~1/10 appropriate amount, utilize spray-drier to spray in the loft drier again, becoming powder through under the fast dewatering, or utilizing freeze drier under high vacuum and very low temperature, to carry out lyophilization, ground back powdering thing again to becoming powder; Perhaps, further extraction liquid is made capsule or ingot sheet, it uses tablet machine to break into ingot shape made meal or uses capsule machine to charge into the capsulae vacuus inner sealing automatically.
Publication number is that the Chinese patent of CN1799573 has been introduced a kind of collection and Chinese traditional patent medicine production methods of controlling the fresh flower leave of insomnia, at the peanut results eve, be ready to pulverizer or squeezing machine etc. as early as possible, after peanut is plucked, remove the impurity such as Huang Ye in the fresh peanut branches and leaves immediately, through operations such as cleaning, pulverizing or squeezings, make liquid or solid-state Chinese patent medicine.
Publication number is the method that the Chinese patent of CN101712669 has been introduced separation and purification luteolin in a kind of Pericarppium arachidis hypogaeae; adopt ultrasonic-assisted extraction; because the equipment of ultrasonic extraction can only be bench-scale testing all, is to be used for the large-scale production luteolin.
In sum, the acquisition of luteolin has chemical synthesis and natural matter extraction method, and chemical synthesis complex process, cost are higher, owing to introduced catalyzer and other compositions, and the generation by product, the removal of impurity is very difficult, and security of products becomes a major issue.Natural matter extracts main with Pericarppium arachidis hypogaeae, Japanese Honeysuckle and the higher vegetable material of some other content of luteolin.The raw material that extracts luteolin at present also is not applied to materials such as peanut root, stem, leaf, the utilization of peanut root mainly is a trans-resveratrol, the utilization of cauline leaf all is some crude extracts, not specific to which effective constituent, with low content of technology, added value is low, does not involve the extraction and the utilization of luteolin.Extracting luteolin with peanut root, stem, leaf the like waste is an extremely valuable technology.
Summary of the invention
The technical solution used in the present invention comprises: with peanut root, stem, leaf, shell is material, through cleaning impurity elimination, pulverizing, with ethanolic soln extraction, filtration, decolouring, concentrating under reduced pressure, reusable heat water precipitation, filtration, filtrate, concentrating under reduced pressure, use resin absorption, ethanol elution then,, obtain the thick product of luteolin the elutriant concentrating under reduced pressure, thick product is molten through alcohol, thin up, recovery ethanol, crystallization, recrystallization, makes the higher luteolin product of purity.
The invention provides a kind of method of utilizing peanut root, stem, leaf, shell to extract luteolin, step comprises:
(1) collection of peanut root, stem, leaf, shell: select fine day to gather ripe collection period at peanut, after peanut is taken, remove the impurity such as earth on the root, stem and leaf, under the sun, dry or 40~50 ℃ of oven dry down, can not stack retting, bake out temperature can not be higher than 60 ℃; Pericarppium arachidis hypogaeae dries or dries after taking out Semen arachidis hypogaeae;
(2) pulverize raw material to 20~40 orders, 1: 15 (M/V) adds 75% ethanol, heating and refluxing extraction 3h to press solid-liquid ratio, filter and obtain extracting solution, filter residue is pressed solid-liquid ratio, and 1: 10 (M/V) adds 75% extraction using alcohol 1.5h, filters, merging filtrate is evaporated to syrupy shape;
(3) concentrated solution is by volume added 5 parts of boiling water, stir, be cooled to below 10 ℃, filter, filtrate is heated to 50 ℃, uses activated carbon decolorizing, filters concentrating under reduced pressure;
(4) concentrated solution KLFC-150 macroporous resin adsorption, and use 75% ethanol elution, collect the elutriant that contains the luteolin component;
(5) the concentrating under reduced pressure elutriant obtains the thick product of luteolin;
(6) the thick product of luteolin repeats (4) (5) step, obtains the luteolin product of higher degree;
(7) the luteolin product that (6) are obtained 75% dissolve with ethanol adds and the isopyknic hot water of ethanol, and ethanol is reclaimed in underpressure distillation, and surplus liquid cooling but back is left standstill 48h under 4 ℃, obtain the luteolin crystallization; Surplus liquid is concentrated into 1/3 volume, leaves standstill 24h under 4 ℃, carries out crystallization, obtains the luteolin crystallization, merges to collect the luteolin crystallization;
(8) crystallization that (7) are obtained is according to the method recrystallization of (7) 1~2 time, and surplus liquid is concentrated into 1/3 volume, leaves standstill the 24h recrystallization once under 4 ℃, merges 2 crystallizations, and vacuum-drying obtains high-purity luteolin.
In a specific embodiments, extract material for shining the dry peanut root.
In another embodiment, extract material for drying Folium Arachidis hypogaeae.
In another embodiment, extract material for drying peanut stem.
In another embodiment, extract material for drying Pericarppium arachidis hypogaeae.
In another embodiment, extracting material is the mixture that dries complete stool peanut root, stem, leaf.
In another embodiment, extracting material is the mixture that dries complete stool peanut root, stem, leaf, shell.
In above-mentioned each scheme, serve as to extract material with the little seed peanut varieties of agricultural university, all material is dry product, and wherein the decolouring of the extract of stem, leaf, root, stem and leaf mixture, root, stem and leaf shell mixture need repeat 2 times.
Advantage of the present invention is:
1, extract luteolin with peanut root, stem, leaf waste as raw material, cost of raw and processed materials is extremely low, and production cost is very low, is the problem of a utilization of waste material, also has active effect to preserving the ecological environment.
2, peanut root, stem, leaf are renewable resources, and raw material sources are abundant, and the industrialization cost is very low, can produce huge economic benefit and social benefit.
3, in present method with ethanol as extracting solvent and eluting solvent, avoided the use of noxious solvent, environmental protection, security is good, impurity such as the bad noxious solvent of products obtained therefrom obtain the approval of domestic and international market easily.
4, purifying process is simple, and equipment requirements is low, and the solvent usage quantity is few, the yield height.
5, utilization of the present invention can improve the economic benefit of peanut cultivation, can play active promoting function for the development of peanut industry, has reduced the production cost of luteolin simultaneously, for the widespread use of luteolin provides the raw material guarantee.
Embodiment:
Below, the present invention will be further detailed with embodiment, but it is not limited to any or the similar example of these embodiment.
Embodiment 1:
Get the little seed peanut varieties of agricultural university after August 25 results peanut, clip peanut root dries, and is crushed to the powder about 10 orders, get absolutely dry peanut root powder 5kg, add 75L 75% ethanol, heating and refluxing extraction 3h, filter, filter residue adds 50L 75% ethanol, and heating and refluxing extraction 1.5h filters, merging filtrate, be evaporated to syrupy shape, get concentrated solution 5.6L, add the 28L boiling water, stir, be cooled to 8 ℃, filter, filtrate is heated to 50 ℃, use activated carbon decolorizing 24h, filter, be evaporated to medicinal extract, collect medicinal extract; Medicinal extract KLFC-150 macroporous resin adsorption is used 75% ethanol elution, collects the elutriant that contains the luteolin component, and the concentrating under reduced pressure elutriant obtains the thick product of luteolin; Thick product KLFC-150 macroporous resin adsorption is used 75% ethanol elution, gets luteolin component 28L, adds 30L waste water, and ethanol is reclaimed in underpressure distillation, continues to be evaporated to about 2L, and 48h is left standstill in the cooling back under 4 ℃, obtain the luteolin crystallization; Surplus liquid is concentrated into 1/3 volume, leaves standstill 24h and carry out crystallization under 4 ℃, obtains the luteolin crystallization, merges to collect the luteolin crystallization; By above method recrystallization 2 times, the vacuum-drying crystallization obtains purity and is 92.5% luteolin 5.94g with luteolin, and yield is 72.1%, and content of luteolin is 0.165% in the peanut root.
Embodiment 2:
Get the little seed peanut varieties of agricultural university after August 25 results peanut, the clip peanut stem dries, and is crushed to the powder about 10~20 orders, get absolutely dry peanut stem powder 5kg, add 75L 75% ethanol, heating and refluxing extraction 3h, filter, filter residue adds 50L 75% ethanol, heating and refluxing extraction 1.5h, filter, merging filtrate is evaporated to syrupy shape, get concentrated solution 5.8L, add the 30L boiling water, stir, be cooled to 8 ℃, filter, filtrate is heated to 50 ℃, uses activated carbon decolorizing 24h, filters, add activated carbon decolorizing 24h again, filter, filtrate decompression is concentrated into medicinal extract, collects medicinal extract; Medicinal extract KLFC-150 macroporous resin adsorption is used 75% ethanol elution, collects the elutriant that contains the luteolin component, and the concentrating under reduced pressure elutriant obtains the thick product of luteolin; Thick product KLFC-150 macroporous resin adsorption is used 75% ethanol elution, gets luteolin component 32L, adds 30L waste water, and ethanol is reclaimed in underpressure distillation, continues to be evaporated to about 2.5L, and 48h is left standstill in the cooling back under 4 ℃, obtain the luteolin crystallization; Surplus liquid is concentrated into 1/3 volume, leaves standstill 24h and carry out crystallization under 4 ℃, obtains the luteolin crystallization, merges to collect the luteolin crystallization; By above method recrystallization 2 times, the vacuum-drying crystallization obtains purity and is 91.8% luteolin 9.59g with luteolin, and yield is 74.2%, and content of luteolin is 0.237% in the peanut stem.
Embodiment 3:
Get the little seed peanut varieties of agricultural university after August 25 results peanut, the clip Folium Arachidis hypogaeae dries, and is crushed to the powder about 10~20 orders, get absolutely dry peanut stem powder 5kg, add 75L 75% ethanol, heating and refluxing extraction 3h, filter, filter residue adds 50L 75% ethanol, heating and refluxing extraction 1.5h, filter, merging filtrate is evaporated to syrupy shape, get concentrated solution 5.8L, add the 30L boiling water, stir, be cooled to 8 ℃, filter, filtrate is heated to 50 ℃, uses activated carbon decolorizing 24h, filters, add activated carbon decolorizing 24h again, filter, filtrate decompression is concentrated into medicinal extract, collects medicinal extract; Medicinal extract KLFC-150 macroporous resin adsorption is used 75% ethanol elution, collects the elutriant that contains the luteolin component, and the concentrating under reduced pressure elutriant obtains the thick product of luteolin; Thick product KLFC-150 macroporous resin adsorption is used 75% ethanol elution, gets luteolin component 32L, adds 30L waste water, and ethanol is reclaimed in underpressure distillation, continues to be evaporated to about 2.5L, and 48h is left standstill in the cooling back under 4 ℃, obtain the luteolin crystallization; Surplus liquid is concentrated into 1/3 volume, leaves standstill 24h and carry out crystallization under 4 ℃, obtains the luteolin crystallization, merges to collect the luteolin crystallization; By above method recrystallization 2 times, the vacuum-drying crystallization obtains purity and is 91.6% luteolin 28.28g with luteolin, and yield is 75.3%, and content of luteolin is 0.688% in the Folium Arachidis hypogaeae.
Embodiment 4:
Get the little seed peanut varieties of agricultural university after August 25 results peanut, the clip Pericarppium arachidis hypogaeae dries, and is crushed to the powder about 10~20 orders, get absolutely dry peanut stem powder 5kg, add 75L 75% ethanol, heating and refluxing extraction 3h, filter, filter residue adds 50L 75% ethanol, heating and refluxing extraction 1.5h, filter, merging filtrate is evaporated to syrupy shape, get concentrated solution 5.8L, add the 30L boiling water, stir, be cooled to 8 ℃, filter, filtrate is heated to 50 ℃, uses activated carbon decolorizing 24h, filters, add activated carbon decolorizing 24h again, filter, filtrate decompression is concentrated into medicinal extract, collects medicinal extract; Medicinal extract KLFC-150 macroporous resin adsorption is used 75% ethanol elution, collects the elutriant that contains the luteolin component, and the concentrating under reduced pressure elutriant obtains the thick product of luteolin; Thick product KLFC-150 macroporous resin adsorption is used 75% ethanol elution, gets luteolin component 32L, adds 30L waste water, and ethanol is reclaimed in underpressure distillation, continues to be evaporated to about 2.5L, and 48h is left standstill in the cooling back under 4 ℃, obtain the luteolin crystallization; Surplus liquid is concentrated into 1/3 volume, leaves standstill 24h and carry out crystallization under 4 ℃, obtains the luteolin crystallization, merges to collect the luteolin crystallization; By above method recrystallization 2 times, the vacuum-drying crystallization obtains purity and is 92.3% luteolin 14.45g with luteolin, and yield is 74.5%, and content of luteolin is 0.358% in the Pericarppium arachidis hypogaeae.
Embodiment 5:
Get the little seed peanut varieties of agricultural university after August 25 results peanut, the whole plant root, stem and leaf is dried, be crushed to the powder about 10~20 orders, get absolutely dry peanut stem powder 5kg, add 75L 75% ethanol, heating and refluxing extraction 3h, filter, filter residue adds 50L 75% ethanol, heating and refluxing extraction 1.5h, filter, merging filtrate is evaporated to syrupy shape, get concentrated solution 5.8L, add the 30L boiling water, stir, be cooled to 8 ℃, filter, filtrate is heated to 50 ℃, uses activated carbon decolorizing 24h, filters, add activated carbon decolorizing 24h again, filter, filtrate decompression is concentrated into medicinal extract, collects medicinal extract; Medicinal extract KLFC-150 macroporous resin adsorption is used 75% ethanol elution, collects the elutriant that contains the luteolin component, and the concentrating under reduced pressure elutriant obtains the thick product of luteolin; Thick product KLFC-150 macroporous resin adsorption is used 75% ethanol elution, gets luteolin component 32L, adds 30L waste water, and ethanol is reclaimed in underpressure distillation, continues to be evaporated to about 2.5L, and 48h is left standstill in the cooling back under 4 ℃, obtain the luteolin crystallization; Surplus liquid is concentrated into 1/3 volume, leaves standstill 24h and carry out crystallization under 4 ℃, obtains the luteolin crystallization, merges to collect the luteolin crystallization; By above method recrystallization 2 times, the vacuum-drying crystallization obtains purity and is 92.2% luteolin 23.81g with luteolin, and yield is 73.8%, and content of luteolin is 0.595% in the Pericarppium arachidis hypogaeae.
Embodiment 6:
Get the little seed peanut varieties of agricultural university after August 25 results peanut, get the whole plant that obtains after the peanut and dry, strip Semen arachidis hypogaeae after peanut dries, Pericarppium arachidis hypogaeae adds in the peanut rhizome leaf, but the whole plant Pericarppium arachidis hypogaeae is crushed to powder about 10~20 orders together, mixes, get mixed powder 5kg, add 75L 75% ethanol, heating and refluxing extraction 3h, filter, filter residue adds 50L 75% ethanol, and heating and refluxing extraction 1.5h filters, merging filtrate, be evaporated to syrupy shape, get concentrated solution 5.8L, add the 30L boiling water, stir, be cooled to 8 ℃, filter, filtrate is heated to 50 ℃, use activated carbon decolorizing 24h, filter, add activated carbon decolorizing 24h again, filter, filtrate decompression is concentrated into medicinal extract, collects medicinal extract; Medicinal extract KLFC-150 macroporous resin adsorption is used 75% ethanol elution, collects the elutriant that contains the luteolin component, and the concentrating under reduced pressure elutriant obtains the thick product of luteolin; Thick product KLFC-150 macroporous resin adsorption is used 75% ethanol elution, gets luteolin component 32L, adds 30L waste water, and ethanol is reclaimed in underpressure distillation, continues to be evaporated to about 2.5L, and 48h is left standstill in the cooling back under 4 ℃, obtain the luteolin crystallization; Surplus liquid is concentrated into 1/3 volume, leaves standstill 24h and carry out crystallization under 4 ℃, obtains the luteolin crystallization, merges to collect the luteolin crystallization; By above method recrystallization 2 times, the vacuum-drying crystallization obtains purity and is 92.7% luteolin 22.75g with luteolin, and yield is 75.6%, and content of luteolin is 0.558% in the mixing material.

Claims (7)

1. method of utilizing peanut root, stem, leaf to extract luteolin, step comprises:
(1) collection of peanut root, stem, leaf: select fine day to gather ripe collection period at peanut, after peanut is taken, remove the earth on the root, stem and leaf, under the sun, dry or dry down at 40~50 ℃;
(2) pulverize raw material to 20~40 orders, press solid-liquid ratio and add 75% ethanol at 1: 15, heating and refluxing extraction 3h filters and obtains extracting solution, and filter residue is pressed solid-liquid ratio and added 75% extraction using alcohol 1.5h at 1: 10, filters, and merging filtrate is evaporated to syrupy shape;
(3) concentrated solution is by volume added 5 parts of boiling water, stir, be cooled to below 10 ℃, filter, filtrate is heated to 50 ℃, and activated carbon decolorizing filters concentrating under reduced pressure;
(4) concentrated solution KLFC-150 macroporous resin adsorption, 75% ethanol elution is collected the component that contains luteolin;
(5) the concentrating under reduced pressure elutriant obtains the thick product of luteolin;
(6) the thick product of luteolin repeats (4) (5) step, obtains the luteolin product of higher degree;
(7) the luteolin product that (6) are obtained 75% dissolve with ethanol adds and the isopyknic hot water of ethanol, and ethanol is reclaimed in underpressure distillation, and surplus liquid cooling but back is left standstill 48h under 4 ℃, obtain the luteolin crystallization; Surplus liquid is concentrated into 1/3 volume, leaves standstill 24h under 4 ℃, carries out crystallization, obtains the luteolin crystallization, merges to collect the luteolin crystallization;
(8) crystallization is according to the method recrystallization of (7) 1~2 time, and surplus liquid is concentrated into 1/3 volume, leaves standstill the 24h recrystallization once under 4 ℃, merges 2 crystallizations, and vacuum-drying obtains high-purity luteolin.
2. the process of claim 1 wherein that starting material are root, stem, the leaf of ripe peanut, it is in time dry that material is wanted, and fresh material can not stack retting or through Temperature Treatment more than 60 ℃.
3. the method for claim 2 is wherein extracted solvent and is 75% ethanol, and ethanol is analytical pure or food grade.
4. the method for claim 3 wherein in the step (3), is extracted and is undertaken by 2 times, and solid-liquid ratio is 1: 15 for the first time, and solid-liquid ratio is 1: 10 for the second time, and extraction time is respectively 3h and 1.5h.
5. the method for claim 4, extracting solution be through concentrating the boiling water that the back adds 5 times of concentrated solution volumes, stirs, cooling, filters with removal impurity.
6. the method for claim 5, wherein step (4) is used the KLFC-150 macroporous resin adsorption, 75% ethanol elution, and repeated the post wash-out 2~3 times.
7. the method for claim 6, wherein will cross the luteolin that obtains behind the post 75% dissolve with ethanol in the step (7), add and the isopyknic hot water of ethanol, ethanol is reclaimed in underpressure distillation, surplus liquid cooling but back is left standstill the 48h crystallization under 4 ℃, after surplus liquid is concentrated into 1/3 volume, leave standstill the 24h crystallization under 4 ℃, merge crystallization, crystallization is adopted with method recrystallization 1~2 time.
CN2011100264699A 2011-01-25 2011-01-25 Method for extracting luteolin from peanut roots, stems, leaves and shells Pending CN102040579A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104529977A (en) * 2014-12-29 2015-04-22 贺州学院 Method for extracting luteolin from water chestnut peel
CN106588848A (en) * 2016-11-15 2017-04-26 浙江工业大学 Method for extracting luteolin from peanut shells
CN107692230A (en) * 2017-10-10 2018-02-16 仲恺农业工程学院 Health products containing resveratrol and cyanidenon and its preparation method and application
CN108623548A (en) * 2018-05-02 2018-10-09 齐齐哈尔大学 The method and its application of hand-type eriodictyol in a kind of separation peanut shell
CN108864023A (en) * 2017-11-02 2018-11-23 昌邑市银江生物科技有限公司 A method of preparing high-purity luteolin

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CN101712669A (en) * 2009-02-13 2010-05-26 河北理工大学 Method for separating and purifying luteolin

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104529977A (en) * 2014-12-29 2015-04-22 贺州学院 Method for extracting luteolin from water chestnut peel
CN106588848A (en) * 2016-11-15 2017-04-26 浙江工业大学 Method for extracting luteolin from peanut shells
CN106588848B (en) * 2016-11-15 2019-10-18 浙江工业大学 The method of luteolin is extracted in a kind of peanut shell
CN107692230A (en) * 2017-10-10 2018-02-16 仲恺农业工程学院 Health products containing resveratrol and cyanidenon and its preparation method and application
CN108864023A (en) * 2017-11-02 2018-11-23 昌邑市银江生物科技有限公司 A method of preparing high-purity luteolin
CN108623548A (en) * 2018-05-02 2018-10-09 齐齐哈尔大学 The method and its application of hand-type eriodictyol in a kind of separation peanut shell

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