CN1066055C - Production method for extracting flavonoid compound extract or powder from bamboo leaf - Google Patents

Abstract

The present invention belongs to a method for producing extracts or powders of flavonoid compounds extracted from plants, particularly to flavonoid compounds extracted from bamboo leaves. In the method, bamboo leaves are used as raw materials, and the bamboo leaves are treated by extraction, concentration, separation, refining or re-drying to obtain the product. The product contains a large quantity of bamboo leaf flavone glucoside, plant phenolic acid, anthraquinone, terpene lactone and other compounds. The preparation has the functions of high free radical resistance, oxidation resistance, senescence resistance, blood fat lowering, etc. The preparation has typical bamboo fragrance, and the preparation can be widely applied to functional foods and medicinal health-care products for all old people. The preparation is treated in hot reflux extraction by using lower alcohol with low concentration as solvent, and is refined by liquid-liquid extraction with middle-grade alcohol. The preparation has the characteristics of safe and convenient production process, easy control, high flavone extracting rate, high purity, etc., and the preparation is suitable for large-scale industrial production.

Description

From Folium Bambusae, extract the production method of flavonoid compound extract or powder

The present invention relates to a kind of production method of from plant, extracting flavone compound, especially from from Folium Bambusae, extracting the production method of flavonoid compound extract or powder.

Biological flavone extensively is present in plant kingdom, is many medium-height grass the effective elements of the medicines.Except extract the flavonoid preparation from Folium Ginkgo, French Cortex Pini, the Japanese Cortex Eucommiae, the biological flavone that Radix Puerariae, Radix Glycyrrhizae, Fructus Crataegi, Folium Camelliae sinensis, Folium Kaki, Folium Pini and Strobilus Pini, Cortex cinnamomi japonici (Ramulus Cinnamomi), Cortex Albiziae, lycii radicis,cortex stem and leaf, Herba Dendrobii, Cordyceps, the Radix Polygoni Multiflori, Pericarpium Citri Reticulatae, Fructus Schisandrae Chinensis, Fructus Jujubae, Pericarppium arachidis hypogaeae, rice root, eggplant bar etc. include all has exploitation and is worth.With current production with use largest ginkgetin to be example, its production technology is roughly following 3 types:

(1) steam distillation: after Folium Ginkgo drying, pulverizing, 100～120 ℃ of steam distillations after the distillate cooling, with non-polar macroporous resin (or other adsorbents) absorption, are used ethanol elution then, and evaporate to dryness promptly gets the powdery crystallization.This method equipment is simple, but extraction ratio is low, now seldom adopts.

(2) organic solvent extraction: this is present domestic and international most popular method, and the patent of its extraction process also more [extracting the method for flavone compound from Folium Ginkgo, Li Zhaolong, Chinese herbal medicine, 1992,14 (6): 5-6] can reduce two kinds of forms.A kind of is to prepare crude extract: Folium Ginkgo drying, pulverizing back are extracted with organic solvent (as ethanol or acetone), behind filtration, the concentrating under reduced pressure recovery solvent, promptly get ginkgo biloba extract.This method production equipment is simple, product yield height (about 12～14%), but contain a large amount of impurity, and being brownish black usually, the general flavone content of goods is 7～10%.Another kind is the preparation extract: at a basic enterprising one-step refining of crude extract, process for purification commonly used has these class methods usually: liquid～liquid extraction (is for example used dichloromethane, chloroform, petroleum ether or benzene defat; Or with butanone, acetone-butanone or ethyl acetate extraction), the sedimentation method (with ammonia or Lead oxide hydrate precipitation) and absorption～analytic method (adsorbents adsorb such as usefulness macroporous resin, kieselguhr or silica gel, ethanol elution).Again by anhydrous sodium sulfate drying, filtration, distilling under reduced pressure remove desolvate after, get final product extract.Be generally the yellowish-brown powder, yield is about 1～3%, and general flavone content is about 20～26%.

(3) supercritical fluid extraction: over nearly 10 years, the effective medicinal components that extracts in natural plants with this technology more and more receives publicity, and it is compared with above-mentioned technology, has extraction efficiency height, no solvent residue, active component is difficult for being decomposed and advantage such as destruction.European patent EP 0308675 (1988) has been reported the method with effective ingredient in the supercritical carbon dioxide extraction Folium Ginkgo, domesticly also does a lot in this respect in recent years, but is in the laboratory research stage mostly, does not see the report that industrial applications is arranged.

Bamboo is grass family (Poaceae) Bambusoideae (Bambusoideae) perennial evergreen plant, is a kind of popular medicine, food dual purpose plant.Bamboo widely distributes in Southeast Asia, and China is one of producing region, center of world's bamboo, existing bamboo kind kind more than 300, more than 6,000 ten thousand mu of bamboo grove areas.The medical care effect of bamboo is familiar with by China working people already, " book on Chinese herbal medicine is looked for the truth " said: " Folium Bambusae carries according to book; the cool heart delays spleen, clearing away phlegm quenches the thirst; for control part of the body cavity above the diaphragm housing the heart and lungs ailment said due to cold or exposure dysphoria with smothery sensation, cough with dyspnea dyspnea with rapid and short breath, the diseases such as the sound of vomiting haematemesiss, all apoplexy infantile convulsion of vomitting, nothing but because of it gently can be separated, hot strongly fragrant, the sweet energy that can loose delays spleen, cold can be gone into the heart, tremble with fear and can treat hot event ear ".Herba Lophatheri and phyllostachys nigra (lodd.ex lindl.) munro var.henonis (miff.) spapf et rendle drop are exactly the traditional simply heat and toxic materials clearing away medicine of the traditional Chinese medical science.The bamboo whole body is precious, is one of plant of having use value most of the world today.But in the comprehensive utilization of bamboo, the research and development of Folium Bambusae obviously lags behind, depolarization a spot of medicinal and edible beyond, basically in a state of nature.In recent years, the inventor has carried out systematic research to the effective ingredient and the biological activity thereof of Folium Bambusae, find to contain abundant phenoloids such as flavone, anthraquinone analog compound, terpene lactone, immunocompetence polysaccharide, extraordinary aminoacid (δ-oxylysine) and manganese, zinc, ferrum, selenium and other trace elements in the Folium Bambusae, wherein flavone compound is its main functional component.The contained flavone compound of Folium Bambusae all is flavone glycoside basically, and considerable part is a carbon glycosides flavone, as orientin xyloside, Lutonaretin, 4 '-methoxyl group-apigenin-8-C-glucoside etc.

Studies show that Folium Bambosae extract (Ebl) has good free radical resisting, antioxidation and activity of fighting against senium.A large amount of studies show that Ebl has the very strong removing reactive oxygen free radical and the ability of stopping nitrosation reaction; Can significantly induce vigor, the inhibition lipid peroxidation of aged mouse endogenous antioxidase system (SOD and GSH-Px) and remove the peroxidating product; Can significantly strengthen resisting fatigue and the anti-stress ability of mice; Ebl can significantly reduce the concentration of rat serum triglyceride and T-CHOL, increases the HDL-cholesterol concentration, reduces the LDL-cholesterol concentration, suppresses the increase of rat body weight.Zooperal result shows that the Ebl blood fat reducing is identical with Folium Ginkgo extract (Egb) with the effect of inducing endogenous SOD vigor, suppresses lipid peroxidation and induces the effect of GSH-Px vigor obviously to be better than Egb.In addition, from Folium Bambusae, do not detect harmful components or antinutritional factor as yet.Acute toxicity test shows, the LD of Ebl per os ₅₀＞10g/kg body weight can be considered actual nontoxic; Salmonella reversion test shows that Ebl does not have mutagenicity.Thus, Ebl is a kind of healthy ingredient of biological flavone safely and efficiently, can be widely used in the control of functional food and multiple old degenerative disease.

The objective of the invention is to utilize the Folium Bambusae that china natural resources is very abundant and effectively developed as yet, provide that a kind of technology is easy, extraction ratio is high, the production method of from Folium Bambusae, extracting flavonoid compound extract or powder that process is easy to control, pollution-free, be suitable for large-scale industrial production.

From Folium Bambusae, extract the production method of flavonoid compound extract or powder, it is characterized in that: be raw material with the Folium Bambusae, Folium Bambusae is cleaned, oven dry, broken, with low concentration (20-40%, concentration expressed in percentage by volume) lower alcohol (methanol or ethanol) is a solvent, with 1: the solid-to-liquid ratio of 10-15 (percentage by weight) hot reflux was extracted 1-2 hour, extracting solution concentrates back physics roguing, reuse medium alcohol (butanols or amylalcohol) liquid-liquid extraction, after the extract concentrating under reduced pressure reclaimed solvent, adding low amounts of water changeed molten, becomes flavonoid compound extract, or, promptly make the flavone compound powder again through vacuum or spray drying.

The present invention is achieved in that

Folium Bambusae → clean → oven dry → fragmentation → ethanol～aqueous solution hot reflux extraction → filtration → concentrating under reduced pressure → static flocculation → separation roguing → n-butyl alcohol fractional extraction → concentrating under reduced pressure reclaims solvent → hot water changes molten → concentrating under reduced pressure → (extractum) → vacuum or spray drying → Folium Bambosae flavone powder

The technical essential of this invention is according to the compositing characteristic of Folium Bambosae flavone compounds and physicochemical property (good hydrophilicity and heat stability), adopts ethanol water disposable thermal reflux, extract; According to impurity flocculation and precipitation characteristic under certain condition, use the physical method for separation roguing; Use the n-butyl alcohol fractional extraction then, reclaim solvent, after the water commentaries on classics is molten, get extractum, be drying to obtain powder again.Technology is simple and direct, is easy to control; The equipment less investment, good separating effect, extraction ratio height; Organic solvent-free is residual, quality of finished product good; That whole process is not used is poisonous, harmful reagent and strong acid and strong base, essentially no " three wastes " discharging, and composing environment pollutes.Technology of the present invention is applicable to continuous production in enormous quantities.

The present invention makes long-term depleted Folium Bambusae obtain deep development, both realized the whole strain utilization of bamboo, by a kind of biological flavone new resources of originating wide, that high-quality is cheap are provided for society, it is significant that the mankind's aging, tumor and cardiovascular diseases etc. are moved back the type prevention and treatment of diseases.

The technology point of Folium Bambusae total flavones preparation is as follows:

(1) the Folium Bambusae raw material can be the dried Folium Isatidis of the scattered bamboo or the bamboo that grows thickly, is good with the kind (as henon bamboo, phyllostachys bambusoides, Phyllostachys pubescens Mazei ex H.de Lebaie, food in one's mouth chicken bamboo, propinquity bamboo, Ph. bambusoides, black bamboo, mottled bamboo etc.) of Phyllostachys, and be autumn and winter (9～December) ideal collection period.

(2) disposable thermal reflux, extract.Get the fragment of dried Folium Isatidis, with the alcoholic solution of 1: 10～15 solid-liquid ratios, 20～40% concentration) hot reflux extraction 1～2hr, the cycle is short, the hold facility rate is low, it is more complete to extract.In view of the popularity of Folium Bambusae raw material and cheap price, this disposable extraction method is most economical, reasonable method.

(3) physics method roguing.Extract solution of bamboo leaves is concentrated to about 1: 1 volume (being that the 1kg cured leaf gets the concentrated solution about 1kg), in the static process of cooling naturally, macromole impurity that includes and part Polyphenols composition flocculate, natural subsidence, method with centrifugalize, filter pressing or vacuum filtration is removed, and has good clarifying effect.This physics roguing method has been saved production cost greatly than the precipitate with ethanol or the clarification of other chemical methodes of routine, and the harmful effect of having avoided chemical reagent may bring extract quality.

(4) the refining employing n-butyl alcohol liquid～liquid extraction method of Folium Bambosae flavone.Because n-butyl alcohol has good dissolubility and selectivity to the Folium Bambosae flavone glucoside, its boiling point is higher, at room temperature not volatile in addition, and proportion is little, be easy to separate and reclaim, and nontoxic, harmless.Carry out the extraction of effective degree with n-butyl alcohol, flavone extraction ratio height, finished product golden yellow color.

(5) behind butanol extraction liquid process concentrating under reduced pressure, the recovery solvent, a spot of hot water of extract reuse changes the melt into flavonoid compound extract, promptly gets the flavone compound powder through vacuum drying or spray drying again.

Folium Bambosae flavone compounds powder with technology preparation of the present invention is yellow powder or yellow crystal granule, have tangible Folium Bambusae fragrance, general flavone content is 24～30%, the overwhelming majority is a flavone glycoside, wherein contain a considerable amount of carbon glycosides flavone, as orientin xyloside, Lutonaretin and 4 '-methoxyl group-apigenin-8-C-glucoside etc.Other compositions also have plant phenolic acid, anthraquinone, terpene lactone, nitrogen-containing compound, soluble sugar and mineral etc.

Embodiment 1: the dried Folium Isatidis 1kg of henon bamboo (Phyllostachy nigra var.henonis (Bean) Stapf exRendle), become the extraction pot of putting into 20L behind the thick sheet about 10 orders with crusher in crushing, the ethanol 12kg of adding 30% soaks 1hr, reflux 1.5hr.Crude extract (about 10kg) is gone into concentrating under reduced pressure in the vacuum concentrator (reclaiming solvent simultaneously) after filtering, discharging when being concentrated into volume and being the 1L left and right sides, static 8hr, vacuum filtration is removed impurity, clear liquid is used n-butanol extraction with volume, and three times (the n-butyl alcohol water in advance is saturated, 40～50 ℃ of insulations extract, stir 0.5～1hr) at every turn, merge n-butyl alcohol and go into concentrating under reduced pressure recovery solvent in the vacuum concentrator mutually, extract changes molten with hot water, become extractum after being evaporated to finite concentration, or the spray-dried again 25g yellow powder that gets, its general flavone content is 28%

The dried Folium Isatidis of embodiment 2:2kg phyllostachys bambusoides (Phyllostachy bambusoides Sieb.Et Zucc), be broken into thick sheet about 10 orders and put into the extraction pot of 50L, the ethanol 30kg of adding 35%, soak 0.5hr, reflux 1hr, put into storage tank behind the extracting liquid filtering, be concentrated into final volume with vacuum concentrator in batches and be about 2L, static 6hr, impurity is removed in centrifugalize, clear liquid merges the n-butyl alcohol phase with the n-butanol extraction of 2 times of volumes 2 times, and concentrating under reduced pressure reclaims solvent, extract is after the hot water commentaries on classics is molten, be evaporated to proportion and become extractum greater than 1.12 backs, or get the 45g yellow powder through vacuum drying again, general flavone content is 27.6%.

Claims (1)

1, from Folium Bambusae, extracts the production method of flavonoid compound extract or powder, it is characterized in that: be raw material with the Folium Bambusae, with Folium Bambusae clean, oven dry, fragmentation, methanol or ethanol with 20～40% concentration expressed in percentage by volumes are solvent, solid-liquid percentage by weight hot reflux with 1: 10～15 was extracted 1～2 hour, extracting solution concentrates back physics roguing, reuse butanols or amylalcohol liquid～liquid extraction, after the extract concentrating under reduced pressure reclaims solvent, add low amounts of water and change molten, become flavonoid compound extract, or, promptly make the flavone compound powder again through vacuum or spray drying.