CN105175376A - Method for extracting luteolin from Laifeng crossostephium leaves - Google Patents
Method for extracting luteolin from Laifeng crossostephium leaves Download PDFInfo
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- CN105175376A CN105175376A CN201510702760.1A CN201510702760A CN105175376A CN 105175376 A CN105175376 A CN 105175376A CN 201510702760 A CN201510702760 A CN 201510702760A CN 105175376 A CN105175376 A CN 105175376A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
- C07D311/30—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/40—Separation, e.g. from natural material; Purification
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Abstract
The invention relates to a method for extracting luteolin from Laifeng crossostephium leaves. The method includes the step A of enzymolysis, the step B of alcohol leaching, the step C of microwave extraction, the step D of filtering, the step E of concentration and the step F of cooling. The method is low in process condition requirement and reasonable in process, the extraction process is unique, the method is suitable for industrialized production conditions, and the extraction efficiency is high; meanwhile, devices are simple, the manufacturing cost is low, and the method is easy to apply and popularize.
Description
Technical field
The present invention relates to a kind of method extracting luteolin from the fragrant chrysanthemum in Laifeng County.
Background technology
Luteolin: chemical name: 3', 4', 5,7-Luteolin, another name: cyanidenon, cyanidenon, English name Luteolin, chemical formula: C15H10O6, molecular weight: 286.23, density: 1.654g/cm3, fusing point: 330 DEG C, boiling point: 616.1 DEG C of at760mmHg, flash-point: 239.5 DEG C, vapour pressure: 9.03E-16mmHgat25 DEG C.Physical behavior: yellow needles, fusing point 328-330 DEG C.Be slightly soluble in water, tool slightly acidic, dissolve in basic solution, stable under normal condition.Luteolin (luteolin) is a kind of natural flavone compounds, is present in various plants.There is multiple pharmacologically active, as anti-inflammatory, antianaphylaxis, antitumor, antibacterial, antiviral etc., be clinically mainly used in cough-relieving, eliminate the phlegm, anti-inflammatory, Cardiovarscular, treatment " amyotrophic lateral sclerosis ", SARS, hepatitis etc.
Luteolin, the form mainly with glucosides is present in various plants, and these plants are higher with Herba Dracocephali Integrifolii, capsicum, Wild Chrysanthemum, Japanese Honeysuckle, purple perilla content.There is antibechic and phlegm-dispelling functions.According to current research, respiratory symptom cough, expectoration, to pant, all relevant with chronic airway inflammation.As bronchial asthma, chronic obstructive pulmonary disease, chronic pharyngitis, rhinallergosis etc. cause cough, expectoration, pant, all be considered to relevant with the inflammatory infiltration of local, the existence of inflammation, make the immunne response of air flue chaotic, patient often occurs that airway reactivity increases.First the means for the treatment of should eliminate the chronic inflammatory diseases infiltration of air flue.Conventional glucocorticosteroid at present, to eliminate airway inflammation.But the side effect of glucocorticosteroid is more, unsuitable prolonged application.Research shows, luteolin suppresses scavenger cell phosphorylation, suppresses the activity of transcription factor NF-kB, and the scavenger cell that lipopolysaccharides (LPS) can be suppressed to induce produces cytokine IL-6, TNF-a.Latter two cytokine plays the part of very important role in inflammation mechanism, is the sensitive indicator of reflection degree of inflammation.Luteolin can also improve IFN-γ, reduces specificity Ig-E, reduces the infiltration of eosinophilic granulocyte.In addition, luteolin, except anti-inflammatory, anti-allergic effects, also has and suppresses PDE, anti-SARS, HIV virus characteristic, and its reason is suppress the activity of SARS virus Pre-S protein, thus stops it to enter host cell.Be used for the treatment of the chronic cough that COPD, bronchial asthma and chronic pharyngitis, rhinallergosis etc. cause.
Dendranthema indicum is feverfew Dendranthema indicum Dendranthemaindicume (L1) DesMonl1var1aromaticumQ1H1L1iuet1S1E1Zhang, the dry capitulum of var1nov1, originate in Shennongjia in Hubei, be distributed in the open field of height above sea level more than 2000 meters on the sunny side, it is a new variant of composite family Chrysanthemum, complete stool has special strong fragrance, Dendranthema indicum sample picks up from Shennongjia, Hubei Province in October, 2004, feverfew Dendranthema indicum Dendranthemaindicum (L1) DesMonl1var1aromaticumQ1H1LiuetS1E1Zhang is accredited as by medicine academy, HuNan college of traditional Chinese medicine identification and assessment of Chinese medicines teaching and research room professor Chen Keli, the dry capitulum of var1nov1.
The diseases such as Dendranthema indicum is used for anti-curing cold by Mountain Area of Western Hubei Province, have a headache, bacillary dysentery, enteritis, constipation, coronary heart disease and hypertension.Its essential oil or medicinal extract are used for the aspects such as medicine, beverage, cigarette and makeup.Lu Jinqing, He Jun, kingdom are bright etc., and people once studied the chemical composition of Dendranthema indicum dried flower essential oil, therefrom identified multiple terpenoid; Gong Fujun etc. are the isolation identification compounds such as robinin, palmitinic acid, lauric acid, daucosterol, robinin 2 rhamnoglucoside, luteolin 272O2 β 2 glucoside, luteolin from Dendranthema indicum.
The fragrant chrysanthemum of Dragon Lord, as a kind of colored veriety with Mountain Area of Western Hubei Province characteristic, is not generally planted, the few places that its place of production mainly concentrates on Shennongjia and bestows favour at home.Bestowing favour, is the important planting area of the fragrant chrysanthemum of Dragon Lord in history, has plantation tradition for many years, has establishing in large scale especially in the east of Sichuan mountain area, and the fragrant chrysanthemum of Dragon Lord has become now local main characteristic and spent one of veriety.
Teng Sheng spices company of Laifeng County planted experimentally from 2012 plants the fragrant chrysanthemum of Dragon Lord, utilize the petal budding technology of its uniqueness, the long technology of fertilizer speed, the planting technologies such as interval mastery soil, successfully plant successfully fragrant chrysanthemum in height above sea level 600-1000 rice low altitude area, it is strong that its fragrant chrysanthemum is bright-colored, fragrance is fresh and sweet, and chrysanthemum head circle is evenly large, output is high, and pharmaceutical use is high.The fragrant chrysanthemum of Teng Sheng spices company plantation is from odour characteristics, mouthfeel, using value, and fragrant chrysanthemum has certain difference with Dragon Lord, becomes and has self-character---and " the fragrant chrysanthemum in Laifeng County ".
" the fragrant chrysanthemum in Laifeng County " that this technology is conceived to the plantation of area, Laifeng County is raw material, volatile for " the fragrant chrysanthemum in Laifeng County " unique fresh and sweet note composition, the features such as easy change, microwave radiation, the modern non-heat-flash technique means such as cellulase treatment, produce from the gradient of " the fragrant chrysanthemum in Laifeng County " full flavor compound and carry out " the fragrant chrysanthemum in Laifeng County " high-valued and industrialization key technology research with finger print identification two aspect systems of full flavor compound in a deep going way, exploitation high added value " the fragrant chrysanthemum in Laifeng County " characteristic perfumed product, and realize industrialization production and apply, eat raw and the transformation of simple processed goods to high added value intensely processed products from simple to realize " the fragrant chrysanthemum in Laifeng County ", improve " the fragrant chrysanthemum in Laifeng County " commodity value, drive " the fragrant chrysanthemum in Laifeng County " industrial chain extension and increase plantation family income, reduce field stockpiling of unsold product, increase agricultural performance, promote the higher value application level of local characteristic agricultural byproducts resource.Meanwhile, by the intensive processing product of " the fragrant chrysanthemum in Laifeng County ", obvious for this provincial characteristics distinguishing products are pushed to the whole nation, pushed the whole world to.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method extracting luteolin from the fragrant chrysanthemum in Laifeng County.
Technical scheme of the present invention is: a kind of method extracting luteolin from the fragrant chrysanthemum in Laifeng County, is characterized in that comprising the following steps:
A. enzymolysis
In extractor, add the fragrant chrysanthemum in Laifeng County, water, cellulase, zytase, B-dextranase and polygalacturonase; Water add-on is 1-10 times of the fragrant chrysanthemum weight in Laifeng County, and auxiliary material add-on is the per-cent of the fragrant chrysanthemum weight in Laifeng County: cellulase 0.1-1%, zytase 0.1-1%, B-dextranase 0.3-3%, polygalacturonase 0.3-3%; Controlled enzymatic hydrolysis temperature 35-55 degree, starts stirring, enzymolysis time: 1-5 hour;
B. alcohol leaching
In extractor, add 5-12 times of alcohol immersion of the fragrant chrysanthemum weight in Laifeng County, 2-24 hour;
C. microwave extraction
Control extractor temperature 50-95 degree, microwave power is under 100-500kw condition, extracts 1-3 hour;
D. filter
Obtain filtrate with 100-300 order sock filtration, storage tank is preserved, and filter residue adds 3-8 times of ethanol, again extracts 2-6 hour at extractor, obtains filtrate with 100-300 order sock filtration, and merging filtrate storage tank is preserved;
E. concentrate
After filtrate being left standstill 6-24 hour, enter thickener and concentrate, temperature controls at 60-70 degree, and vacuum tightness concentrates at 0.8-0.95, stops when material dry matter content is greater than 55%;
F. cool
Material is cooled to normal temperature, obtains the luteolin medicinal extract that solid matter relative content is greater than 55%.
A kind of method extracting luteolin from the fragrant chrysanthemum in Laifeng County of the present invention, is characterized in that comprising the following steps:
A. enzymolysis
In extractor, add the fragrant chrysanthemum in Laifeng County, water, cellulase, zytase, B-dextranase and polygalacturonase; Water add-on is 1-10 times of the fragrant chrysanthemum weight in Laifeng County, and auxiliary material add-on is the per-cent of the fragrant chrysanthemum weight in Laifeng County: cellulase 0.1-1%, zytase 0.1-1%, B-dextranase 0.3-3%, polygalacturonase 0.3-3%; Controlled enzymatic hydrolysis temperature 35-55 degree, starts stirring, enzymolysis time: 1-5 hour;
B. alcohol leaching
In extractor, add 5-12 times of alcohol immersion of the fragrant chrysanthemum weight in Laifeng County, 2-24 hour;
C. microwave extraction
Control extractor temperature 50-95 degree, microwave power is under 100-500kw condition, extracts 1-3 hour; Microwave extraction system used: adopt the maet-6 microwave extraction system that Shanghai Jing Qiao drying plant factory produces;
D. filter
Obtain filtrate with 100-300 order sock filtration, storage tank is preserved, and filter residue adds 3-8 times of ethanol, again extracts 2-6 hour at extractor, obtains filtrate with 100-300 order sock filtration, and merging filtrate storage tank is preserved;
E. concentrate
After filtrate being left standstill 6-24 hour, enter thickener and concentrate, temperature controls at 60-70 degree, vacuum tightness concentrates at 0.8-0.95, first reclaims ethanol, ethanol is recovered to ethanol storage tank, when concentrated solution alcohol concentration meter detects, time not containing ethanol, ethanol reclaims and stops; Then proceed moisture evaporation, stop when material dry matter content is greater than 55%;
F. cool
Material is cooled to normal temperature, obtains the luteolin medicinal extract that solid matter relative content is greater than 55%.
A kind of method extracting luteolin from the fragrant chrysanthemum in Laifeng County of the present invention, the fragrant chrysanthemum main chemical compositions in Laifeng County used, research shows, in " the fragrant chrysanthemum in Laifeng County ", main component has luteolin, chlorogenic acid, linarin, amino acid, polysaccharide, flavonoid, chlorogenic acid, the compositions such as volatile essential oil, measure the volatile component of " the fragrant chrysanthemum in Laifeng County ", and the general flavone content of more different chrysanthemum and volatile oil yield, result shows, in " Laifeng County fragrant chrysanthemum " general flavone content and volatile oil content all higher, cis-oxidation phantol (21.84%) is had in volatile oil, spathulenol (4.25%), her Elemenum (8.23%), her eudesmol (13.90%), 2 are had in Static Headspace analysis, 3. butyleneglycol (5.69%), only. phellandrene (31.05%), Paracymene (38.08%), three. phantol (7.63%), linalool oxide (29.38), the basal component of dry " the fragrant chrysanthemum in Laifeng County " is mainly: dry-matter 80% ~ 90%, protein 1% ~ 1.8%, carbohydrate 6.3% ~ 10.8%, robust fibre 0.6% ~ 1.7%, fat 0.1%, calcium 0.2 ~ 0.5%, the mineral element such as iron, potassium, manganese, zinc of phosphorus 0.05% and abundant vitamin A, B1, B2, C and trace." the fragrant chrysanthemum in Laifeng County " is about containing the ethereal oil of 0.015% (dry product content is about 0.15%), mainly aromatic compound, although content is little, but these compounds constitute its distinctive local flavor and physiological function composition, be at present to one of focus that " the fragrant chrysanthemum in Laifeng County " physiologically active ingredient is studied.Main function composition in " the fragrant chrysanthemum in Laifeng County " specifically can be divided into following a few class:
Anti-oxidant activity.Luteolin and chlorogenic acid are the main components in " the fragrant chrysanthemum in Laifeng County ", and resistance of oxidation is also stronger; Flavonoids, is mainly present in leaf, stem and crust, with flavonoid, flavonols and anthocyan for representative; Phenylpropanoid glycoside, is mainly present in leaf, stem, comprises monomer and the derivatives thereof such as coffic acid, forulic acid, sinapinic acid; Steroidal compounds and nitrogenous compound.
" the fragrant chrysanthemum in Laifeng County " has its special Physiological Properties, " Laifeng County fragrant chrysanthemum " and " the fragrant chrysanthemum in Laifeng County " deep processed product has effect of bactericidal antiphlogistic, flat liver improving eyesight, loose wind step-down, the diseases such as fragrant chrysanthemum is used for anti-ly curing cold by Mountain Area of Western Hubei Province, have a headache, bacillary dysentery, enteritis, constipation, coronary heart disease and hypertension.
A kind of method extracting luteolin from the fragrant chrysanthemum in Laifeng County of the present invention, processing condition require low, rational technology; Extraction process is created, and be applicable to commercial production conditions, extraction efficiency is high, and equipment is simple simultaneously, and low cost of manufacture, applies easy.
Raw material used in the inventive method, equipment are common common raw material, equipment, avoid the dependence for expensive raw materials, instrument in commercial process, greatly reduce production cost; Easily, cuttage, group training, output is high, moderate, convenient sources, and following resource is secure for the fragrant chrysanthemum plantation in Laifeng County.Use the fragrant chrysanthemum in Laifeng County as raw material; both the utilising efficiency in Laifeng County's fragrant chrysanthemum winter had been substantially increased; improve the added value of the fragrant chrysanthemum in Laifeng County; break away from again for the dependence of other material as raw materials such as Reseda odorata, Semen arachidis hypogaeae shells; market can be alleviated to other raw-material heavy demand; can make full use of the fragrant chrysanthemum in discarded Laifeng County again simultaneously, protect the plant resourceses such as Reseda odorata.
The inventive method is simple to operate, resin chromatography filtering technique need not be used, also do not need precision instrument or automatic equipment, the fragrant resourceful township and village enterprises of chrysanthemum can produce in Laifeng County, this greatly reduces the production cost of luteolin, simplifies production process.
The present invention's reagent used is chemical reagent that is nontoxic, cheap, volume production, and the routine techniques that ripe reagent can be utilized in whole process to reclaim, this greatly reduces to environmental emission waste.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
Embodiment 1: a kind of method extracting luteolin from the fragrant chrysanthemum in Laifeng County of the present invention, comprises the following steps:
A. enzymolysis
In extractor, add the fragrant chrysanthemum in Laifeng County, water, cellulase, zytase, B-dextranase and polygalacturonase; Water add-on is 1 times of the fragrant chrysanthemum weight in Laifeng County, and auxiliary material add-on is the per-cent of the fragrant chrysanthemum weight in Laifeng County: cellulase 0.1%, zytase 0.1%, B-dextranase 0.3%, polygalacturonase 0.3%; Controlled enzymatic hydrolysis temperature 35 degree, starts stirring, enzymolysis time: 1 hour;
B. alcohol leaching
In extractor, add 5 times of alcohol immersion of the fragrant chrysanthemum weight in Laifeng County, 2 hours;
C. microwave extraction
Control extractor temperature 50 degree, microwave power is under 100kw condition, extracts 1 hour; Microwave extraction system used: adopt the maet-6 microwave extraction system that Shanghai Jing Qiao drying plant factory produces;
D. filter
Obtain filtrate with 100 order sock filtration, storage tank is preserved, and filter residue adds 3 times of ethanol, again extracts 2 hours at extractor, obtains filtrate with 100 order sock filtration, and merging filtrate storage tank is preserved;
E. concentrate
After filtrate is left standstill 6 hours, enter thickener and concentrate, temperature controls at 60 degree, and vacuum tightness concentrates 0.8, first reclaims ethanol, ethanol is recovered to ethanol storage tank, and when concentrated solution alcohol concentration meter detects, time not containing ethanol, ethanol reclaims and stops; Then proceed moisture evaporation, stop when material dry matter content is greater than 55%;
F. cool
Material is cooled to normal temperature, obtains the luteolin medicinal extract that solid matter relative content is greater than 55%.
Embodiment 2: a kind of method extracting luteolin from the fragrant chrysanthemum in Laifeng County of the present invention, comprises the following steps:
A. enzymolysis
In extractor, add the fragrant chrysanthemum in Laifeng County, water, cellulase, zytase, B-dextranase and polygalacturonase; Water add-on is 10 times of the fragrant chrysanthemum weight in Laifeng County, and auxiliary material add-on is the per-cent of the fragrant chrysanthemum weight in Laifeng County: cellulase 1%, zytase 1%, B-dextranase 3%, polygalacturonase 3%; Controlled enzymatic hydrolysis temperature 55 degree, starts stirring, enzymolysis time: 5 hours;
B. alcohol leaching
In extractor, add 12 times of alcohol immersion of the fragrant chrysanthemum weight in Laifeng County, 24 hours;
C. microwave extraction
Control extractor temperature 95 degree, microwave power is under 500kw condition, extracts 3 hours; Microwave extraction system used: adopt the maet-6 microwave extraction system that Shanghai Jing Qiao drying plant factory produces;
D. filter
Obtain filtrate with 300 order sock filtration, storage tank is preserved, and filter residue adds 8 times of ethanol, again extracts 6 hours at extractor, obtains filtrate with 300 order sock filtration, and merging filtrate storage tank is preserved;
E. concentrate
After filtrate is left standstill 24 hours, enter thickener and concentrate, temperature controls at 70 degree, and vacuum tightness concentrates 0.95, first reclaims ethanol, ethanol is recovered to ethanol storage tank, and when concentrated solution alcohol concentration meter detects, time not containing ethanol, ethanol reclaims and stops; Then proceed moisture evaporation, stop when material dry matter content is greater than 55%;
F. cool
Material is cooled to normal temperature, obtains the luteolin medicinal extract that solid matter relative content is greater than 55%.
Embodiment 3: a kind of method extracting luteolin from the fragrant chrysanthemum in Laifeng County of the present invention, comprises the following steps:
A. enzymolysis
In extractor, add the fragrant chrysanthemum in Laifeng County, water, cellulase, zytase, B-dextranase and polygalacturonase; Water add-on is 5 times of the fragrant chrysanthemum weight in Laifeng County, and auxiliary material add-on is the per-cent of the fragrant chrysanthemum weight in Laifeng County: cellulase 0.5%, zytase 0.5%, B-dextranase 1.5%, polygalacturonase 1.5%; Controlled enzymatic hydrolysis temperature 45 degree, starts stirring, enzymolysis time: 2.5 hours;
B. alcohol leaching
In extractor, add 8 times of alcohol immersion of the fragrant chrysanthemum weight in Laifeng County, 12 hours;
C. microwave extraction
Control extractor temperature 75 degree, microwave power is under 300kw condition, extracts 1.5 hours; Microwave extraction system used: adopt the maet-6 microwave extraction system that Shanghai Jing Qiao drying plant factory produces;
D. filter
Obtain filtrate with 200 order sock filtration, storage tank is preserved, and filter residue adds 5.5 times of ethanol, again extracts 4 hours at extractor, obtains filtrate with 200 order sock filtration, and merging filtrate storage tank is preserved;
E. concentrate
After filtrate is left standstill 15 hours, enter thickener and concentrate, temperature controls at 65 degree, and vacuum tightness concentrates 0.9, first reclaims ethanol, ethanol is recovered to ethanol storage tank, and when concentrated solution alcohol concentration meter detects, time not containing ethanol, ethanol reclaims and stops; Then proceed moisture evaporation, stop when material dry matter content is greater than 55%;
F. cool
Material is cooled to normal temperature, obtains the luteolin medicinal extract that solid matter relative content is greater than 55%.
Embodiment 4: a kind of method extracting luteolin from the fragrant chrysanthemum in Laifeng County of the present invention, comprises the following steps:
A. enzymolysis
In extractor, add the fragrant chrysanthemum in Laifeng County, water, cellulase, zytase, B-dextranase and polygalacturonase; Water add-on is 8 times of the fragrant chrysanthemum weight in Laifeng County, and auxiliary material add-on is the per-cent of the fragrant chrysanthemum weight in Laifeng County: cellulase 0.8%, zytase 0.8%, B-dextranase 2%, polygalacturonase 2%; Controlled enzymatic hydrolysis temperature 50 degree, starts stirring, enzymolysis time: 4 hours;
B. alcohol leaching
In extractor, add 10 times of alcohol immersion of the fragrant chrysanthemum weight in Laifeng County, 20 hours;
C. microwave extraction
Control extractor temperature 80 degree, microwave power is under 400kw condition, extracts 2 hours; Microwave extraction system used: adopt the maet-6 microwave extraction system that Shanghai Jing Qiao drying plant factory produces;
D. filter
Obtain filtrate with 250 order sock filtration, storage tank is preserved, and filter residue adds 7 times of ethanol, again extracts 5 hours at extractor, obtains filtrate with 250 order sock filtration, and merging filtrate storage tank is preserved;
E. concentrate
After filtrate is left standstill 20 hours, enter thickener and concentrate, temperature controls at 68 degree, and vacuum tightness concentrates 0.92, first reclaims ethanol, ethanol is recovered to ethanol storage tank, and when concentrated solution alcohol concentration meter detects, time not containing ethanol, ethanol reclaims and stops; Then proceed moisture evaporation, stop when material dry matter content is greater than 55%;
F. cool
Material is cooled to normal temperature, obtains the luteolin medicinal extract that solid matter relative content is greater than 55%.
Embodiment 5: a kind of method extracting luteolin from the fragrant chrysanthemum in Laifeng County of the present invention, comprises the following steps:
A. enzymolysis
In extractor, add the fragrant chrysanthemum in Laifeng County, water, cellulase, zytase, B-dextranase and polygalacturonase; Water add-on is 4 times of the fragrant chrysanthemum weight in Laifeng County, and auxiliary material add-on is the per-cent of the fragrant chrysanthemum weight in Laifeng County: cellulase 0.4%, zytase 0.4%, B-dextranase 1%, polygalacturonase 1%; Controlled enzymatic hydrolysis temperature 38 degree, starts stirring, enzymolysis time: 2 hours;
B. alcohol leaching
In extractor, add 8 times of alcohol immersion of the fragrant chrysanthemum weight in Laifeng County, 5 hours;
C. microwave extraction
Control extractor temperature 70 degree, microwave power is under 150kw condition, extracts 1.2 hours; Microwave extraction system used: adopt the maet-6 microwave extraction system that Shanghai Jing Qiao drying plant factory produces;
D. filter
Obtain filtrate with 150 order sock filtration, storage tank is preserved, and filter residue adds 4 times of ethanol, again extracts 3 hours at extractor, obtains filtrate with 150 order sock filtration, and merging filtrate storage tank is preserved;
E. concentrate
After filtrate is left standstill 8 hours, enter thickener and concentrate, temperature controls at 68 degree, and vacuum tightness concentrates 0.85, first reclaims ethanol, ethanol is recovered to ethanol storage tank, and when concentrated solution alcohol concentration meter detects, time not containing ethanol, ethanol reclaims and stops; Then proceed moisture evaporation, stop when material dry matter content is greater than 55%;
F. cool
Material is cooled to normal temperature, obtains the luteolin medicinal extract that solid matter relative content is greater than 55%.
Embodiment 6: a kind of method extracting luteolin from the fragrant chrysanthemum in Laifeng County of the present invention, comprises the following steps:
A. enzymolysis
In extractor, add the fragrant chrysanthemum in Laifeng County, water, cellulase, zytase, B-dextranase and polygalacturonase; Water add-on is 6 times of the fragrant chrysanthemum weight in Laifeng County, and auxiliary material add-on is the per-cent of the fragrant chrysanthemum weight in Laifeng County: cellulase 0.6%, zytase 0.6%, B-dextranase 2.1%, polygalacturonase 2.1%; Controlled enzymatic hydrolysis temperature 39 degree, starts stirring, enzymolysis time: 4 hours;
B. alcohol leaching
In extractor, add 7 times of alcohol immersion of the fragrant chrysanthemum weight in Laifeng County, 20 hours;
C. microwave extraction
Control extractor temperature 80 degree, microwave power is under 400kw condition, extracts 2.5 hours; Microwave extraction system used: adopt the maet-6 microwave extraction system that Shanghai Jing Qiao drying plant factory produces;
D. filter
Obtain filtrate with 300 order sock filtration, storage tank is preserved, and filter residue adds 6 times of ethanol, again extracts 5 hours at extractor, obtains filtrate with 300 order sock filtration, and merging filtrate storage tank is preserved;
E. concentrate
After filtrate is left standstill 22 hours, enter thickener and concentrate, temperature controls at 66 degree, and vacuum tightness concentrates 0.89, first reclaims ethanol, ethanol is recovered to ethanol storage tank, and when concentrated solution alcohol concentration meter detects, time not containing ethanol, ethanol reclaims and stops; Then proceed moisture evaporation, stop when material dry matter content is greater than 55%;
F. cool
Material is cooled to normal temperature, obtains the luteolin medicinal extract that solid matter relative content is greater than 55%.
Claims (2)
1. from the fragrant chrysanthemum in Laifeng County, extract a method for luteolin, it is characterized in that comprising the following steps:
A. enzymolysis
In extractor, add the fragrant chrysanthemum in Laifeng County, water, cellulase, zytase, B-dextranase and polygalacturonase; Water add-on is 1-10 times of the fragrant chrysanthemum weight in Laifeng County, and auxiliary material add-on is the per-cent of the fragrant chrysanthemum weight in Laifeng County: cellulase 0.1-1%, zytase 0.1-1%, B-dextranase 0.3-3%, polygalacturonase 0.3-3%; Controlled enzymatic hydrolysis temperature 35-55 degree, starts stirring, enzymolysis time: 1-5 hour;
B. alcohol leaching
In extractor, add 5-12 times of alcohol immersion of the fragrant chrysanthemum weight in Laifeng County, 2-24 hour;
C. microwave extraction
Control extractor temperature 50-95 degree, microwave power is under 100-500kw condition, extracts 1-3 hour;
D. filter
Obtain filtrate with 100-300 order sock filtration, storage tank is preserved, and filter residue adds 3-8 times of ethanol, again extracts 2-6 hour at extractor, obtains filtrate with 100-300 order sock filtration, and merging filtrate storage tank is preserved;
E. concentrate
After filtrate being left standstill 6-24 hour, enter thickener and concentrate, temperature controls at 60-70 degree, and vacuum tightness concentrates at 0.8-0.95, stops when material dry matter content is greater than 55%;
F. cool
Material is cooled to normal temperature, obtains the luteolin medicinal extract that solid matter relative content is greater than 55%.
2., according to a kind of method extracting luteolin from the fragrant chrysanthemum in Laifeng County according to claim 1, it is characterized in that comprising the following steps:
A. enzymolysis
In extractor, add the fragrant chrysanthemum in Laifeng County, water, cellulase, zytase, B-dextranase and polygalacturonase; Water add-on is 1-10 times of the fragrant chrysanthemum weight in Laifeng County, and auxiliary material add-on is the per-cent of the fragrant chrysanthemum weight in Laifeng County: cellulase 0.1-1%, zytase 0.1-1%, B-dextranase 0.3-3%, polygalacturonase 0.3-3%; Controlled enzymatic hydrolysis temperature 35-55 degree, starts stirring, enzymolysis time: 1-5 hour;
B. alcohol leaching
In extractor, add 5-12 times of alcohol immersion of the fragrant chrysanthemum weight in Laifeng County, 2-24 hour;
C. microwave extraction
Control extractor temperature 50-95 degree, microwave power is under 100-500kw condition, extracts 1-3 hour; Microwave extraction system used: adopt the maet-6 microwave extraction system that Shanghai Jing Qiao drying plant factory produces;
D. filter
Obtain filtrate with 100-300 order sock filtration, storage tank is preserved, and filter residue adds 3-8 times of ethanol, again extracts 2-6 hour at extractor, obtains filtrate with 100-300 order sock filtration, and merging filtrate storage tank is preserved;
E. concentrate
After filtrate being left standstill 6-24 hour, enter thickener and concentrate, temperature controls at 60-70 degree, vacuum tightness concentrates at 0.8-0.95, first reclaims ethanol, ethanol is recovered to ethanol storage tank, when concentrated solution alcohol concentration meter detects, time not containing ethanol, ethanol reclaims and stops; Then proceed moisture evaporation, stop when material dry matter content is greater than 55%;
F. cool
Material is cooled to normal temperature, obtains the luteolin medicinal extract that solid matter relative content is greater than 55%.
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