CN103146476A - Green extraction technique capable of comprehensively and efficiently utilizing sophora flower bud - Google Patents
Green extraction technique capable of comprehensively and efficiently utilizing sophora flower bud Download PDFInfo
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- CN103146476A CN103146476A CN 201210566992 CN201210566992A CN103146476A CN 103146476 A CN103146476 A CN 103146476A CN 201210566992 CN201210566992 CN 201210566992 CN 201210566992 A CN201210566992 A CN 201210566992A CN 103146476 A CN103146476 A CN 103146476A
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Abstract
The green extraction technique capable of comprehensively and efficiently utilizing sophora flower bud mainly comprises the following steps:1), extracting sophora flower bud essential oil; 2), extracting rutin; 3), extracting quercetin; 4) extracting pigment; 5), extracting sophora flower bud polysaccharide; 6) extracting sophora flower bud protein; and 7) preparing sophora flower bud dregs. In a production process, sophora flower bud resources are fully utilized to the greatest degree, raw materials can be fully converted into production, and pollution is nearly avoided. Compared with the technique extracting single component from the sophora flower bud, comprehensive benefits of the sophora flower bud is greatly played, and economical and social sustainable development is achieved.
Description
Technical field
The present invention relates to the green extractive technique that a kind of comprehensive high-efficiency utilizes sophora bud resource.
Background technology
The sophora bud is the bud of leguminous plants Chinese scholartree Sophora japonica, main product in Henan, the ground such as Shandong, Shanxi, Shaanxi, Anhui, Hebei, Jiangsu, also existing scale plantation of the ground such as Ningxia, Gansu in recent years, also there is large-area plantation in Vietnam.Main violaguercitrin-rutin (rutin), the triterpenoid saponin of containing in the sophora flower flower bud, as: red bean saponin(e (azukisaponin) I, II, V, soybean saponin (soyasaponin) I, III, kaikasaponin (kaikasaponin) I, II, III.Also contain flavones ingredient as Quercetin (quercetin), Isorhamnetol (isorhamnetin), Isorhamnetol-3-rutinoside (isorhamnetin-3-rutinoside), kaempferol-3-rutinoside (kaempferol-3-rutinoside), Flos Sophorae Immaturus first element (14%) etc.Contain again trochol (betulin), sophoradiol (sophoradiol).Also contain the phytosterin compounds such as Flos Sophorae Immaturus second element (1.25%) and Flos Sophorae Immaturus the third element (0.35%) in the sophora flower flower bud.low polarity component in sophora flower has lauric acid (lauric acid), dodecenoic acid (dodecenoic acid), tetradecanoic acid (myristic acid), tetradecenoic acid (tetradecenoic acid) tetradecadienoic acid (teradecadienoic acid), palmitinic acid (palmitic acid), hexadecylenic acid (hexadecenoicacid), stearic acid (stearic acid), octadecadienoic acid (octadecadienoic acid), ten make carbon trienic acid (octadecatrienoic acid), the lipid acid such as eicosanoic acid (arachidic acid) and the β-sitosterol (composition such as β-sitosterol) and tannin.Moisture content 78 grams in every 100 gram sophora bud fresh goods in addition, protein 3.1 grams, fatty 0.7 gram, carbohydrate 15 grams, 8.3 milligrams of calcium, 69 milligrams, phosphorus, 3.6 milligrams of iron, 0.04 milligram of carotene, vitaminB10 .04 milligram, 0.18 milligram of Lin Suanna Vitamin B2 Sodium Phosphate, 6.6 milligrams of nicotinic acids, 66 milligrams of vitamins Cs.
The function of the sophora bud cures mainly cooling blood for hemostasis, clearing liver-fire.Be used for having blood in stool, hemorrhoid blood, bloody flux, uterine bleeding, haematemesis, bleeding from five sense organs or subcutaneous tissue, the hot hot eyes of liver, headache is dizzy, treatment psoriatic, the treatment tuberculosis of cervical lymph nodes, treatment heat furuncle etc.Dietary function has cooling blood for hemostasis, and sophora flower is mainly used in the hemorrhage illness that belongs to blood-head, can coordinate garden burnet treatment bottom hemorrhage as have blood in stool, hematuria, hemorrhoid blood, coordinate Herba Agrimoniae, Rhizome of Lalang Grass treatment top is hemorrhage as spitting of blood, bleeding from five sense organs or subcutaneous tissue etc.; Reduce blood pressure, the contained violaguercitrin (rutin) of preventing apoplectic sophora flower is to have the VITAMIN that strengthens capillary resistance, can strengthen vessel wall elasticity, improve the toughness of capillary vessel, the hyperpietic is had the effect that prevents rupture of blood vessel in brain, but preventing apoplectic there is remarkable hypotensive activity.The sophora bud is widely used in sophora bud dripping pill, sophora bud fermented type low sugar yoghurt, sophora bud antioxidant, sophora bud hairdressing sun cream, sophora bud Jiangya Granula, sophora bud bee honey health-care beverage, sophora bud biscuit, sophora bud health tea, Compound Huaimi capsules, chrysanthemum sophora bud capsule, the loose treatment of sophora bud aluminite infectious hepatitis, sophora bud dried rhizome of rehmannia soup treatment erythroderma desquamativum, the loose treatment of compound sophora bud psoriatic, sophora bud infusion treatment lithangiuria, the loose treatment of sophora bud pig courage grasserie.Sophora bud dyestuff is a kind of natural vegetable dye, not only can do the pigment of food, can also do the dyestuff of textiles.Sophora bud water logging agent can obviously be shortened hemorrhage and the clotting time, promotes after charcoal processing that Blood clotting is stronger; Its decocting liquid has the minimizing myocardial consumption of oxygen, the effect of cardiac function protecting.Separately to trichophyton, permitted blue achorion, Du's big belly budlet spore tinea bacterium difficult to understand, ulotrichy budlet spore tinea bacterium, starlike slave and block the dermatophytes such as bacterium in various degree restraining effect is arranged.
Producer all can only extract a kind of composition of violaguercitrin from the sophora bud both at home and abroad at present, has wasted other compositions in the sophora bud.The present invention's comprehensive high-efficiency from the sophora bud extracts other effective constituent, takes full advantage of sophora bud resource, and when extracting rutin, synchronous high-efficiency has extracted sophora bud oil, Quercetin, sophora flower-bud pigment, sophora bud polysaccharide, sophora bud albumen, sophora flower bud dregs etc., and accomplished to clean extraction.
sophora bud oil is a kind of low-pole composition in the sophora bud, mainly contain ketone, alcohol, acid, sterol, phenol, aldehyde, ester, alkane, the compound such as alkene and heterocycle, as stearic acid, tetradecanoic acid, linolic acid, linolenic acid, eicosanoic acid, behenic acid and phytol etc., comprise 1, 9, 12-three oxygen-4, the 6-diamino basic ring tetradecane-5-thioketones (20.58%), 8-heptadecene (26.358%), [S-(R*, S*)]-5-(1, 5-dimethyl-4-hexenyl)-2-methyl isophthalic acid, 3-cyclohexadiene (12.093%), caryophyllene (11.969%), palmitinic acid (9.05%), 2-methoxyl group-3-(2-propenyl) phenol (8.460%), 9, 12, 15-octadecatrienol (7.05%), (Z, Z)-9, 12-octadecadienoic acid (6.85%) and β-sitosterol (6.11%) etc.Has antibacterial antioxygenation.Sophora flower-bud pigment is a kind of glycoside, and glycosyl is glucose or rhamnosyl, and glycoside is flavones or flavonol.Flavones, flavonol are yellow crystal, and flavanone, flavanonol are colourless crystallization, and be all water-soluble.Sophora flower-bud pigment is safe, tone is natural, and has certain nutrition and pharmacological action.Sophora bud polysaccharide not only has very strong reducing power, and ultra-oxygen anion free radical, hydroxyl radical free radical are all had removes preferably ability, is expected to as natural antioxidants and food functionality composition and is developed and applied.The sophora flower polysaccharide component mainly is comprised of rhamnosyl, fructose, pectinose and wood sugar, and molecular weight is 2-～11kD, specific rotation+40～130 °.Sophora bud albumen is a kind of vegetable-protein of pure natural, contains 16 seed amino acids, energy vessel softening, dilution thrombus, increase human capillary vessel's permeability.Hypertension, hyperlipidemia, diabetes are had preferably treatment and prophylactic effect, but also nourishing the liver, protect liver, anti-cancer can be manufactured various medicine, also can increase as foodstuff additive the protein content of its food.Sophora bud protein is mainly gluten, white protein and sphaeroprotein etc., the viscosity of this protein is poor, gluten-free type, with the bean protein similar, form from amino acid, quality is better than rice, wheat and maize, sophora bud albumen is similar to the nutrition of egg protein, contain 19 abundant seed amino acids, wherein the amino acid of 8 kinds of needed by human composition is reasonable, proportioning is suitable, meets or surpass Food and Argriculture OrganizationFAO and the World Health Organization to essential amino acids content set quota in food proteins.Sophora flower bud dregs is that sophora bud processing after ripening is later through selected, pulverizing, and the processing such as oven dry are made, and have higher nutritive value.Have effect clearing heat and detoxicating, promoting blood circulation and removing blood stasis, help digest absorption, prevention diarrhoea, rich vitamin, crude protein, crude fat and robust fibre etc. are good fodder additives (ox chicken and duck rabbit pig) and organic fertilizer.Use this product can make the flavescence of livestock and poultry fat color, improve its commodity utilization ratio rate, use this product can reduce feed cost, improve efficiency of feed utilization.Its aminoacids content is only second to soya-bean cake, is better than wheat, and is more advanced with the nutritive value of comparing with other products of price.
Summary of the invention
The extraction of the first sophora bud oil: with wet distillation, obtain distilled oil after the sophora bud is pulverized.With the volatile component meal that contains in the sophora bud, soak moistening after, straight fire heating retort or pass into steam distillation, the volatile component in medicinal material is taken out of with wet distillation, collects distillate after condensation, layering obtains oil reservoir.Worked simultaneously to kill enzyme in still-process, killed two birds with one stone.The ultimate principle of this law is according to Dalton's law, and the steam stagnation pressure of insoluble also chemically inert liquid mixture, equal each component saturation vapour pressure (being dividing potential drop) sum at this temperature mutually.Although therefore the boiling point of each component itself is higher than the boiling point of mixed solution, when the dividing potential drop summation equaled normal atmosphere, liquid mixture namely came to life and is distilled out.
The extraction of the second rutin: domestic traditional alkali extraction and acid precipitation extracts rutin from the sophora bud.In the solvent batch tank, configuration alkali lye, after alkali lye pH value is 13, show that solvent prepares.The sophora bud powder that screening is good is packed in extractor.The tap water of 35 ℃ is put into extractor, flow out water as clear as crystal after (effluent liquid B bottom is standby), prepare diacolation, ooze out liquid pH value and be and stopped diacolation at 13 o'clock.Stop after adding hydrochloric acid to be neutralized to pH value 3～4 in percolate, standing, acid is washed in press filtration, drying.Pressing filtering liquid C transfers neutral, and is concentrated, obtains Industrial Salt, purified waste water, obtained Chemicals.
The extraction of the 3rd Quercetin: extract in good rutin and contain Quercetin, add reagent A to extract, obtain Quercetin.Because Quercetin and rutin are flavonoid compound, chemical property is similar, has also proposed Quercetin when extracting rutin.
The 4th sophora flower-bud pigment extracts: extract the water liquid B of rutin with membrane concentration, the mixture that is precipitated as polysaccharide and albumen that obtains is the crude product pigment after filtered liquid is concentrated.The crude product pigment obtains the elaboration pigment after processing with reagent D, and the residuum after processing obtains compd E with silica gel column chromatography.
The extraction of the 5th sophora bud polysaccharide: process the mixture of sophora bud polysaccharide and albumen with polysaccharide and albumen initial gross separation with solvent F, the Crude polysaccharides that obtains is with water dissolution, process with trypsinase+Sevage method again, be hydrolyzed major part in conjunction with albumen and floating preteins, be conducive to the stripping of polysaccharide material, also reduced the stickiness of polysaccharide soln simultaneously, be equipped with again the Sevage method, deproteinated efficient is high, and the loss of polysaccharide is little, is conducive to being further purified of vacuum concentration and sophora bud polysaccharide
The extraction of the 6th sophora bud albumen: the crude protein that has separated polysaccharide filters with the sepharose filtration method after with water dissolution, obtains the albumen elutriant, and is concentrated
The preparation of the 7th sophora flower bud dregs: the sophora bud slag that has extracted rutin washes with water to neutral post-drying.
Description of drawings
Fig. 1 sophora bud integrated extraction technique schema
Fig. 2 rutin high-efficient liquid phase chromatogram
Fig. 3 Quercetin high-efficient liquid phase chromatogram
Fig. 4 pigment high-efficient liquid phase chromatogram
Embodiment
Get 1000Kg sophora bud powder and drop in retort, soak 2～5h, open steam valve, heated and boiled, distillation constantly obtains distillate, collects oil phase after layering, so repeats 1～2 time.Obtain sophora bud volatile oil and the dregs of a decoction.Put into tap water in the solvent batch tank, load weighted 50Kg NaOH is slowly added in the solvent batch tank, the limit edged stirs, until institute add solute dissolve fully be 13 with pH test paper survey pH after, show that solvent has prepared, stand-by; According to upper method give successively 2#, 3#, that 4# solvent batch tank prepares solvent is stand-by.The sophora bud powder that screening is good is evenly slowly packed in extractor, should note meal is contained in pot bottom thin whizzer, each centrifugal 20 minutes, washing approximately 1 hour during tinning.Centrifuge washing is complete, closes whizzer.The material that centrifuge washing is good is sent into drying room.The material that centrifuge washing is good is put into vacuum rotary drying machine, opens drying machine, keeps vacuum tightness-0.08Mpa.Open steam valve, make 40～60 ℃ of dryer temperature retentive control temperature, dry 2.5 hours.Obtain Quercetin 25.8Kg, content 98.4% (UV).
Water liquid B when extracting rutin adopts embrane method to carry out concentrating and separating to pharmaceutical products, compare with traditional concentration techniques such as evaporation, but membrane concentration technique progressively shows the advantage of the aspects such as its technology and economy with its energy-conservation, efficient normal-temperature operation (to heat-sensitive substance without destroying) etc.Therefore consider that suspended substance and macromolecular substance in water liquid B are more, removed suspended substance before entering coarse filtration film system.Simultaneously for the concentrated film of the macromole contaminate subsequent that prevents minute quantity, therefore be provided with rough filtering device before concentrated film.Native system employing polysulfone hollow fiber ultrafiltration membrane system system.Comprise the equipment such as ultra-filtration membrane device, back washing device, gas-washing device.10 of the antipollution PUF8060 polypropylene screen elements that uses under coarse filtration film system employing high pollution environment.Have high strength, withstand voltage, acid and alkali-resistance, antipollution, long service life, filter and adopt external-compression type, can process high concentration material, feed liquid sees through membranous wall from the outside to intermediate filtered under pressure promotes, under squeezing action, film is to internal contraction, and fenestra can ensure filter effect like this apart from only can be more and more less.During backwash, backwash liquor sees through membranous wall from inside hollow fibre and rinses outward, and fenestra is gone out pollutent apart from enlarging, and recovers film properties.Concentrated film unit adopts 9 of the concentrated dedicated film elements of material.Native system adopts special macromolecule material, its surface active layer is fine and close, have the characteristics such as withstand voltage, anti-pollution, easy cleaning, long service life, and can guarantee for a long time the clarity of clear liquid, colloid, suspended particle, turbidity, bacterium, larger molecular organics are had good separating power.Membrane treatment appts adopts the automatic operation scheme of cross flow filter.Cleaning system (CIP) in process of production, feed liquid can be accumulated in the film surface, pollution film layer causes flux to reduce.For recovering membrane flux, must carry out the CIP on-line cleaning.Clean and generally carry out when every batch materials EO.Obtain the thick pigment 98.5Kg of the sophora bud, thick pigment obtains refining pigment 47.3Kg after processing with reagent D, is yellowish brown, maximum absorption wavelength 420nm, be soluble in acetone, chloroform, ether, water insoluble, ethanol demonstrates the characteristic of carotenoid, and is stable to most metal ions, to ph stability, unstable to illumination.
The solid substance that membrane concentration obtains is processed with solvent F, separates to obtain Crude polysaccharides and crude protein.Crude polysaccharides is with water dissolution, then processes with trypsinase+Sevage method.The characteristics of protein sex change in the organic solvents such as trichloroethane, with extracting solution and Sevage Reagent Chloroform: propyl carbinol=5: 1 (V/V) mixes, vibration, centrifugal, the protein after sex change is between extracting solution and Sevage reagent intersection.Then get deproteinated and get polysaccharide liquid and add hydrogen peroxide decolouring, alcohol precipitation filters, and obtains refined sophora flower bud polysaccharide 34.6Kg, surveys content as 94.8% take the phenolsulfuric acid method.The crude protein that has separated polysaccharide adds in the sepharose Filter column after with water dissolution, first with water elution, again with buffer solution elution, collect protein-contg elutriant, add activated carbon decolorizing 30min, filter, concentrating under reduced pressure, obtain refined sophora flower bud albumen 66.2Kg, calculate content, content (mL/mg)=1.45 * A according to experimental formula
280nm-0.74 * A
260nmObtain content 92.4%.Sophora bud slag after the extraction rutin obtains sophora flower bud dregs 548Kg with drinking washing to neutral rear at 70-80 ℃ of dry 8-12h.
Claims (8)
1. a comprehensive high-efficiency utilizes the green extractive technique of sophora bud resource, it is characterized in that, take the sophora bud as raw material, the method is successively through following steps:
(1) extraction of sophora bud volatile oil: the sophora bud is pulverized, and with water soaking, adds the water distillation, collects oil reservoir after the distillate layering that obtains and obtains sophora bud volatile oil.But this method has both obtained volatile oil, the high temperature enzyme that goes out was arranged, prevented the enzymolysis violaguercitrin.
(2) extraction of rutin: extract the dregs of a decoction of volatile oil, prepare rutin with alkali extraction and acid precipitation, taked the promoting agent assisted extraction, regulate suitable potential of hydrogen and extract and precipitate, obtain the higher rutin of quality and yield.The pressing filtering liquid neutralization, concentrated, crystallization is filtered, and obtains Chemicals and distilled water, whole process environmental protection.
(3) extraction of Quercetin: contain Quercetin in the rutin of extraction, process with reagent A, obtain refined rutin and Quercetin.
(4) sophora flower-bud pigment extracts: the water liquid B in extraction rutin process is with membrane concentration, be precipitated thing and water liquid, with the concentrated crude product sophora flower-bud pigment that obtains of water liquid, the crude product sophora flower-bud pigment obtains the elaboration pigment after processing with reagent D, and the resistates that reagent D was processed obtains compd E with silica gel column chromatography.
(5) extraction of sophora bud polysaccharide: the residue after membrane concentration is processed through solvent F, can be with polysaccharide and albumen initial gross separation, and the Crude polysaccharides after separation is processed with trypsinase+Sevag method again, obtains high-quality sophora bud polysaccharide.
(6) extraction of sophora bud albumen: the crude protein that has extracted polysaccharide obtains high-quality sophora bud albumen with the processing of sepharose filtration method.
(7) preparation of sophora flower bud dregs: the sophora bud slag that extracted rutin washs with tap water, until after water lotion is neutrality, press dry, oven dry obtains sophora flower bud dregs.Water lotion transfers water liquid B afterwards neutral and in step (4) to mix, membrane concentration.
2. a kind of comprehensive high-efficiency as claimed in claim 1 utilizes the green extractive technique of sophora bud resource, it is characterized in that, in step (1), wet distillation should be carried out in extractor or still kettle, should repeat to distill 1～2 time.
3. a kind of comprehensive high-efficiency as claimed in claim 1 utilizes the green extractive technique of sophora bud resource, it is characterized in that, the reagent in step (3) should be the dissolving Quercetin and do not dissolve rutin, and safety non-toxic.
4. a kind of comprehensive high-efficiency as claimed in claim 1 utilizes the green extractive technique of sophora bud resource, it is characterized in that, in step (4), membrane concentration should have higher thickening efficiency, and agents useful for same D should have certain polarity, and compd E is saponins compound.
5. a kind of comprehensive high-efficiency as claimed in claim 1 utilizes the green extractive technique of sophora bud resource, it is characterized in that, in step (5), solvent F is the mixture of two kinds of reagent, preferably separating polyose and albumen.Trypsinase+Sevag method is processed the strongest to the removing ability of albumen, and the albumen clearance rate can reach more than 90%, and the polysaccharide loss rate also reduces greatly simultaneously, is better than other extracting method.
6. a kind of comprehensive high-efficiency as claimed in claim 1 utilizes the green extractive technique of sophora bud resource, it is characterized in that, in step (6), the sepharose filtration method is a kind of method of utilizing gel that the different separating substances of molecular size is opened, gel itself is a kind of molecular sieve, can separate macrobead and small-particle the same as sieving.Again with in same solvent elution process, macromole can not enter that gel is inner and space along between gel particle is flowed out outside post at first, and small molecules can enter gel inside, and flow velocity is last the outflow outside post slowly, thereby the different material matter of molecular size is separated.Obtain highly purified sophora bud albumen.
7. a kind of comprehensive high-efficiency as claimed in claim 1 utilizes the green extractive technique of sophora bud resource, it is characterized in that, the sophora bud slag in step (7) must wash neutrality with water just can advance the drying room oven dry.
8. as claim 1,2,3,4,5,6,7 described a kind of comprehensive high-efficiencies utilize the green extractive technique of sophora bud resource, it is characterized in that socioeconomic Sustainable development.Not only little to the harmful effect that environment produces in production process, even there is no harmful effect, the more important thing is in the process of producing, farthest take full advantage of sophora bud resource, make starting material fully be converted into product, do not produce pollution as far as possible.Traditional sophora bud extracts just rutin, has wasted other composition, causes a large amount of wastings of resources.Along with illustrating of other activeconstituentss, each constituents is carried out simultaneous extraction, comprehensive utilization, can effectively improve the economic worth of the sophora bud.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103408619A (en) * | 2013-07-31 | 2013-11-27 | 李玉山 | Greening comprehensive utilization technology of flos sophorea immaturus resources |
| CN105315317A (en) * | 2015-10-29 | 2016-02-10 | 南京中医药大学 | Product prepared by heating quercetin and rhamnose as well as preparation method and application thereof |
| CN105647230A (en) * | 2016-03-10 | 2016-06-08 | 常州大学 | Natural Flos Sophorae Immaturus dye extraction method and application of natural Flos Sophorae Immaturus dyes |
| CN114921283A (en) * | 2015-09-30 | 2022-08-19 | 公立大学法人大阪 | Method and apparatus for producing vegetable oil |
| CN116655712A (en) * | 2023-07-31 | 2023-08-29 | 山东省中医药研究院 | Method for rapidly preparing high-purity rutin based on pagodatree flower bud water extract |
-
2012
- 2012-12-24 CN CN 201210566992 patent/CN103146476A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103408619A (en) * | 2013-07-31 | 2013-11-27 | 李玉山 | Greening comprehensive utilization technology of flos sophorea immaturus resources |
| CN103408619B (en) * | 2013-07-31 | 2016-03-16 | 李玉山 | A kind of method of comprehensive utilization of sophora bud resource |
| CN114921283A (en) * | 2015-09-30 | 2022-08-19 | 公立大学法人大阪 | Method and apparatus for producing vegetable oil |
| CN105315317A (en) * | 2015-10-29 | 2016-02-10 | 南京中医药大学 | Product prepared by heating quercetin and rhamnose as well as preparation method and application thereof |
| CN105647230A (en) * | 2016-03-10 | 2016-06-08 | 常州大学 | Natural Flos Sophorae Immaturus dye extraction method and application of natural Flos Sophorae Immaturus dyes |
| CN116655712A (en) * | 2023-07-31 | 2023-08-29 | 山东省中医药研究院 | Method for rapidly preparing high-purity rutin based on pagodatree flower bud water extract |
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Application publication date: 20130612 |