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

Abstract

The present invention pertains to a flavonoid extracted from plants, in particular production process to extract flavonoids from the extract or powder of bamboo. In bamboo as a raw material, by extraction, concentration, separation, purification, and then drying the resulting product, or, it contains a lot of bamboo flavone glycosides, phenolic acids and plant, anthraquinone, terpene lactone compounds. The formulation has an excellent anti-free radical, anti-oxidation, anti-aging and hypolipidemic action, and with a typical aromatic bamboo, can be widely applied to various functional foods and pharmaceutical elderly health products. The preparation is extracted with a lower alcohol, a low concentration of heat at reflux solvent, was purified ~ Intermediate liquid extraction with an alcohol solution. The production process is safe, simple, clean, easy to control, suitable for large-scale industrial production, and also has flavonoids extraction rate, good purity and other characteristics.

Description

Extraction production of flavonoids from the extract or powder of bamboo

The present invention relates to a method for the production of flavonoids extracted from plants, especially from the production of the extraction of flavonoids from the extract or powder of bamboo.

Bioflavonoids widespread in the plant kingdom, is the active ingredient in many Chinese herbal medicine. In addition to flavonoids extracted from the preparation of Ginkgo biloba, French pine bark, other than Japan gutta, kudzu, licorice, hawthorn, tea, persimmon leaves, pine needles and pine real, cinnamon, Albizia, wolfberry root bark of stems and leaves, Dendrobium, Chinese caterpillar fungus, containing the bioflavonoids Radix, orange peel, Schisandra, dates, peanut shells, rice root, eggplant rods, etc. all have development value. In today's largest production and use of flavonoids as an example, its production process is generally the following three types: (1) steam distillation: The Ginkgo biloba dried, crushed, 100 ~ 120 ℃ steam distillation, the distillate was cooled after non-polar macroporous resin (or other adsorbent) is adsorbed, and then eluted with ethanol, evaporated to dryness to obtain powdery crystals. The apparatus is simple, but the extraction rate, is now rarely used.

(2) organic solvent extraction: This is the method most widely used at home and abroad, which patent is greater extraction process [Extraction of flavonoids from Ginkgo leaves, Lizhao Long, herbs, 1992,14 (6): 5 -6], it can be summarized into two forms. One is the preparation of crude extracts of: Ginkgo biloba dried, pulverized and extracted with an organic solvent (e.g. ethanol or acetone), filtered, and concentrated under reduced pressure to recover the solvent, to give the ginkgo extract. This method is simple production equipment, high product yield (about 12 to 14%), but containing a large amount of impurities, typically brownish-black, total flavonoids article is 7 to 10%. Another is to prepare fine extracts: generally further purified by such methods, commonly used method of refining the crude extract on the basis of: - liquid-liquid extraction (e.g. methylene chloride, chloroform, benzene or petroleum ether, defatted; or with butanone, acetone - extracted with ethyl acetate or methyl ethyl ketone), precipitation (with ammonia or lead hydroxide precipitation) and adsorption - analytical method (with a macroporous resin, diatomaceous earth or silica gel adsorbent, eluting with ethanol) . Then dried over anhydrous sodium sulfate, filtered and distilled to remove the solvent under reduced pressure to obtain refined extract. Generally as a tan powder, yield from about 1 to 3%, of the total flavonoid content from about 20 to 26%.

(3) SFE: the past 10 years, the natural extract active ingredients of medicinal plants with more and more attention to the technique, the process described above and which, compared with a high extraction efficiency, no solvent residue, the active ingredient is not easily advantages decomposition and destruction. European Patent EP0308675 (1988) reported a method to extract the active ingredients of gingko leaves with supercritical CO2, also in this country in recent years has done a lot of work, but mostly in the laboratory research stage, there are no reports of industrial applications .

Bamboo is a grass family (Poaceae) Bambusoideae (Bambusoideae) perennial evergreen plant, is a popular drug, and edible plants. In Southeast Asia, bamboo is widely distributed, our country is one of the central areas of the world bamboo, the existing 300 kinds of bamboo, bamboo forest area of ​​over 6,000 acres. Health effects of bamboo has long been recognized for our working people, "Materia Medica truth", saying: "According to the book carrying bamboo, cold heart slow spleen, phlegm thirst quencher for the treatment of coke wind cold Fanre, Keni breathlessness , vomiting hiccup vomiting, all embolism stroke, epilepsy, nothing can be light because the solution, can oct San Yu, Gan can slow spleen, cool to the heart, so cold to heat treatment ears. " Fresh bamboo leaves and pale Xianzhuli is blindly traditional Chinese medicine drug detoxification. Bamboo body is a treasure, is one of the world's plants have the most use value. But in the comprehensive utilization of bamboo, bamboo research and development has lagged far behind, except for a very small amount of medicinal and edible, basically in pristine condition. In recent years, the inventors of the active ingredient of bamboo leaves and biological activity of a systematic study, it was found bamboo leaves are rich in flavonoids and other phenolic compounds, anthraquinone compounds, terpene lactones, immunoactive, special amino acids (delta-hydroxylysine), and manganese, zinc, iron, selenium and other trace elements, wherein the flavonoids are the main functional components. Flavonoids are substantially contained in bamboo flavone glycosides, a considerable portion of flavonoid C-glycosides such as orientin xylosidase, homoorientin, 4'-methoxy - vitexin like.

Studies have shown that ble (Ebl) has excellent anti-free radical, anti-oxidation and anti-aging activity. A number of studies, has strong Ebl Antioxygenation and ability to block the nitrosation reaction; significantly induce the activity of endogenous antioxidant enzymes in aged mice (SOD and GSH-Px), and inhibition of lipid Clear peroxide and peroxide product; significantly enhance the anti-stress and anti-fatigue mice; Ebl significantly reduce the concentration in rat serum triglyceride and total cholesterol, HDL- cholesterol concentration increase, decrease LDL- cholesterol concentration, inhibiting increase in body weight of rats. Animal studies showed that, Ebl lipid lowering effect and induce endogenous SOD activity and Ginkgo biloba extract (Egb) the same, inhibiting lipid peroxidation and GSH-Px activity inducing action was superior to Egb. Further, yet harmful components from the detection or anti-nutritional factors in bamboo leaves. Acute toxicity tests showed, Ebl oral LD50> 10g / kg body weight, may be considered as nontoxic; Ames test showed that, Ebl no mutagenicity. So, Ebl is a safe and effective bioflavonoids health factors, can be widely used in the prevention and treatment of functional foods and a variety of degenerative diseases.

The purpose of the invention is the use of our country is very rich in resources and has not been effective development and utilization of bamboo, to provide a simple process, the extraction rate, the process is easy to control, pollution-free, suitable for large-scale industrial production of extracts from bamboo leaves production of flavonoids in the extract or powder.

Extraction production of flavonoids from the extract powder or bamboo, which is characterized in that: the bamboo as a raw material, the bamboo cleaning, drying, crushing, with low concentrations (20-40%, the volume percentage concentration) in a lower alcohol (methanol or ethanol) as the solvent, the solid-liquid extraction of 1-2 hours 1:10-15 ratio (% by weight) was heated under reflux, the extract was concentrated to physical heteroaryl, then intermediate alcohol (butanol or pentanol) liquid - liquid extraction, the extract was concentrated under reduced pressure to recover the solvent, redissolution small amount of water, to extract flavonoids, or additionally by vacuum or spray drying, i.e. flavonoids obtain powders.

The present invention is achieved: bamboo → washing → drying → crushing → ~ hot aqueous ethanol reflux extraction concentrated under reduced pressure → → → filtration → static flocculation separation undoping → → butanol extraction step to recover the solvent concentrated under reduced pressure hot concentrated → → → redissolution (extract) → → vacuum or spray drying powders EOB technical points of the invention is reduced depending on the composition and characteristics of physicochemical properties of bamboo flavonoids (hydrophilicity and good heat stability), using the one hot aqueous ethanol reflux extraction; the flocculation and precipitation of impurities characteristic under certain conditions, to physically separating heteroaryl; step then extracted with butanol, recovering the solvent, redissolved with water to give the extract, and then dried to obtain a powder. Simple process, easy to control; less equipment investment, separation, and extraction rate; no residual organic solvents, good product quality; the whole process does not use toxic and hazardous reagents, and acid and alkali substantially free "waste" discharge, does not constitute environmental pollution. The process of the invention is suitable for continuous mass production.

The present invention enables long-abandoned bamboo leaves get in-depth development, only to achieve the whole use of bamboo by providing a source for the broad community, bioflavonoids new high-quality low-cost resources, human aging, cancer and cardiovascular disease prevention and treatment of diseases such as type of retirement is important.

Process points total EOB prepared as follows: (1) bamboo leaf stem material can be scattered or clumping bamboo, Phyllostachys to type (such as wool bamboo, Makino, bamboo, bamboo feeding chicken, praecox bamboo, high section of bamboo, black bamboo, owner, etc.) is better, it is the ideal harvest time in autumn and winter (September to December).

(2) a disposable thermal reflux extraction. Dry pieces of leaf taken, by solid-liquid ratio of 1:10 to 15, 20 to 40% ethanol solution concentration) thermal reflux extraction 1 ~ 2hr, short cycle, equipment utilization is low, more complete extraction. Given the breadth and low prices of raw bamboo leaves, the one-time extraction method is the most economical and reasonable method.

(3) physical methods dedoping. Bamboo extract was concentrated to a volume of about 1:1 (i.e. 1kg dried leaves obtained concentrate was approximately 1kg), still in the process of natural cooling, and the portion containing impurities macromolecules polyphenolic component flocculation, sedimentation Nature, by centrifugation, vacuum filtration, or pressure filtration method for removing, having a good refining effect. The physical undoping process than conventional alcohol precipitation, or other chemical clarification methods, saving the cost of production, and avoids the adverse effects of chemical agents may bring the quality of the extract.

(4) purification using EOB butanol solution - liquid extraction. Because butanol solubility and good selectivity for bamboo flavone glycosides, together with its higher boiling point, less volatile at room temperature, the proportion of small, easy separation and recovery, and non-toxic, harmless. It was extracted with n-butanol number of effective, high flavonoid, finished golden color.

(5) n-butanol extract was concentrated under reduced pressure, the solvent is recovered, then a small amount of hot water extracts were redissolved into flavonoid extract, and then to obtain the dried powders of flavonoids in vacuo or spray drying.

Flavonoids in bamboo powder prepared by the inventive technique as a yellow crystalline powder or yellow particles, with a clear aromatic bamboo, total flavonoid content 24 to 30%, most of the flavone glycosides, which contain a significant amount of flavonoid C-glycosides such as orientin xylosidase, homoorientin and 4'-methoxy - vitexin like. There are other components of the plant phenolic, anthraquinone, terpene lactones, nitrogen-containing compounds, soluble sugars and minerals.

Example 1: Mao bamboo (Phyllostachy nigra var.henonis (Bean) Stapf exRendle) of the leaf stem 1kg, with a crusher into coarse mesh sheet into about 10 in an extraction tank 20L, 30% ethanol 12kg soak 1hr, heated to reflux for 1.5hr. The crude extract (about 10kg) was filtered into the vacuum concentrator and concentrated under reduced pressure (while recovering the solvent), concentrated to a volume around the discharge when 1L, 8hr stationary, vacuum filtration removal of impurities, the same volume of supernatant with n and extracted three times with butanol (n-butanol saturated with water beforehand, 40 ~ 50 ℃ heat extraction, each time stirring 0.5 ~ 1hr), the combined butanol phase was concentrated under vacuum to recover the solvent was concentrated at reduced pressure, redissolved in hot water extract , and concentrated under reduced pressure to a certain concentration to the extract, or spray drying and then 25g of a yellow powder having a total flavone content of 28% Example 2: 2kg wallflower (Phyllostachy bambusoides Sieb.Et Zucc) of the leaf stem, broken into about 10 mesh coarse pieces into the extraction tank 50L, 35% ethanol was added 30kg, soaking 0.5hr, heated to reflux for 1 hr, the extract was filtered into a tank, concentrated using a vacuum concentrator to a final batch volume of about after as 2L, still 6 hr, centrifuged to remove impurities, the supernatant with 2 volumes of n-butanol extracted twice, n-butanol phases were combined and concentrated under reduced pressure to recover the solvent, redissolution hot water extract was concentrated under reduced pressure to after a specific gravity greater than 1.12 into extract, and then dried under vacuum, or To give 45g of a yellow powder, 27.6% of total flavonoids.

Claims (1)

1. Production method of extracting flavonoids from the extract or powder of bamboo, which is characterized in that: the bamboo as a raw material, the bamboo cleaning, drying, crushing, with a concentration of 20 percent by volume to 40% methanol or ethanol as solvent extraction 1 to 2 hours in a solid-liquid heated to reflux 1:10 weight percent to 15, the extract was concentrated to physical heteroaryl, then - liquid extraction butanol or pentanol extract was concentrated under reduced pressure recovering the solvent, redissolution small amount of water, to extract flavonoids, or additionally by vacuum or spray drying, i.e. flavonoids obtain powders.