CN106608822A - Method for extracting chlorogenic acid from Laifeng crossostepium leaves - Google Patents
Method for extracting chlorogenic acid from Laifeng crossostepium leaves Download PDFInfo
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- CN106608822A CN106608822A CN201510702778.1A CN201510702778A CN106608822A CN 106608822 A CN106608822 A CN 106608822A CN 201510702778 A CN201510702778 A CN 201510702778A CN 106608822 A CN106608822 A CN 106608822A
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- China
- Prior art keywords
- ethanol
- hours
- crossostephii chinensis
- folium crossostephii
- laifeng county
- Prior art date
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- DPJRMOMPQZCRJU-UHFFFAOYSA-M thiamine hydrochloride Chemical compound Cl.[Cl-].CC1=C(CCO)SC=[N+]1CC1=CN=C(C)N=C1N DPJRMOMPQZCRJU-UHFFFAOYSA-M 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 210000004291 uterus Anatomy 0.000 description 1
- 235000019155 vitamin A Nutrition 0.000 description 1
- 239000011719 vitamin A Substances 0.000 description 1
- 235000010374 vitamin B1 Nutrition 0.000 description 1
- 239000011691 vitamin B1 Substances 0.000 description 1
- 235000019164 vitamin B2 Nutrition 0.000 description 1
- 239000011716 vitamin B2 Substances 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
- 229940045997 vitamin a Drugs 0.000 description 1
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/58—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
Abstract
The invention relates to a method for extracting chlorogenic acid from Laifeng crossostepium leaves. The method comprises the following steps: A, enzymatic hydrolysis; B, alcohol leaching; C, microwave extraction; D, filtering; E, concentration; and F, cooling. The method for extracting chlorogenic acid from Laifeng crossostepium leaves is low in requirements on process conditions, reasonable in process, creative in extraction technology, suitable for industrial production and high in extraction efficiency; and equipment used in the method is simple, low in manufacturing cost and easily practicable for promotion and application.
Description
Technical field
The present invention relates in a kind of Folium Crossostephii Chinensis from Laifeng County chlorogenic acid extracting method.
Background technology
Chlorogenic acid, molecular weight 354.31, density 1.65g/cm3,205-209 DEG C of fusing point, 665 DEG C of boiling point,
245.5 DEG C of flash-point, -37 ° of refractive index.
Chlorogenic acid has wide antibacterial action, but can be inactivated by protein in vivo.It is similar to caffeic acid,
During oral or lumbar injection, the central excitatory of rat can be improved.Can increase rat and mice small intestinal peristalsis and
The tension force of rat uterus.There is choleretic effect, the bile secretion of rat can be promoted.There is sensitization to people, suck
After plant dust containing this product, asthma, dermatitis etc. can occur.
Chlorogenic acid (Chlorogenic acid), is by caffeic acid (Caffeic acid) and quinic acid (Quinic
Acid, QA) depside that generates is plant Jing Folium illicii Lanceolati during aerobic respiration
A kind of phenylpropanoids that sour approach is produced.
Chlorogenic acid has extensive biological activity, and research of the modern science to chlorogenic acid biological activity has been deep into food
The multiple fields such as product, health care, medicine and daily-use chemical industry.Chlorogenic acid is a kind of important bioactive substance, tool
There are antibacterial, antiviral, increase leukocyte, hepatic cholagogic, antitumor, lowering blood pressure and blood fat, removing freely
Base and stimulating central nervous system system etc. are acted on.
Dendranthema indicum is feverfew Dendranthema indicum Dendranthem aindicum e (L1) DesMonl1 var1
Arom aticum Q1H1L1 iuet1S1E1 Zhang, the dry capitulum of var1 nov1 originate in Hubei
Shennongjia, is distributed in the field open on the sunny side of more than 2000 meters of height above sea level, is that of Compositae Chrysanthemum is new
Mutation, Herb have special strong fragrance, and Dendranthema indicum sample in October, 2004 picks up from Shennongjia, Hubei Province,
By medicine academy, HuNan college of traditional Chinese medicine TCD identification, teaching and research room professor Chen Keli is accredited as feverfew Dendranthema indicum
Dendranthem a ind icum(L1)DesMonl1 var1 arom aticum Q1 H1 Liu et S1 E1Zhang,
The dry capitulum of var1 nov1.
Mountain Area of Western Hubei Province by Dendranthema indicum be used for it is anti-cure cold, have a headache, bacillary dysentery, enteritis, constipation, coronary heart disease and height
The diseases such as blood pressure.Its quintessence oil or extractum are used for the aspects such as medicine, beverage, medicated cigarette and cosmetics.Lu Jinqing, what
Bright et al. the chemical composition for once studying Dendranthema indicum dry flower quintessence oil of pretty, kingdom, therefrom identifies multiple terpenoid
Compound；Gong Fujun etc. from Dendranthema indicum isolation identification acacetin, Palmic acid, lauric acid, daucosterol,
The compounds such as 2 rhamnoglucoside of acacetin, 2 glucosides of chlorogenic acid 272O2 β, chlorogenic acid.
Dragon Lord Folium Crossostephii Chinensis are not generally planted at home as a kind of colored veriety with Mountain Area of Western Hubei Province characteristic, its
The place of production is concentrated mainly on Shennongjia and the few places bestowed favour.Bestow favour, be the important plantation of Dragon Lord Folium Crossostephii Chinensis in history
, there is plantation tradition for many years in region, especially has an establishing in large scale in the east of Sichuan mountain area, Dragon Lord Folium Crossostephii Chinensis now into
For one of main characteristic flower veriety in place.
Teng Sheng spice company of Laifeng County planted experimentally plant Dragon Lord Folium Crossostephii Chinensis from 2012, using its unique petal budding technology,
The planting technologies such as the long technology of fertilizer speed, interval mastery soil, successfully in height above sea level 600-1000 rice low altitude areas
Successfully Folium Crossostephii Chinensis are planted in area, and it is strong that its Folium Crossostephii Chinensis is bright-colored, fragrance is fresh and sweet, and Flos Chrysanthemi head circle is big uniform, yield
Height, medical value are high.The Folium Crossostephii Chinensis of Teng Sheng spice company plantation from odor characteristic, mouthfeel, using value, and
Dragon Lord Folium Crossostephii Chinensis have certain difference, become with self-character --- and " Laifeng County's Folium Crossostephii Chinensis ".
It is raw material that this technology is conceived to " Laifeng County's Folium Crossostephii Chinensis " of Laifeng County area plantation, unique for " Laifeng County's Folium Crossostephii Chinensis "
Fresh and sweet note composition is volatile, the features such as easily change, the modern non-heat-flash technology such as microwave radiation, cellulase treatment
Means, produce the finger print identification two with full flavor components from the gradient of " Laifeng County's Folium Crossostephii Chinensis " full flavor components
Aspect system carries out that " Laifeng County's Folium Crossostephii Chinensis " high-valued and industrialization key technology research in a deep going way, and exploitation high added value " is come
Phoenix Folium Crossostephii Chinensis " characteristic aroma product, and realize industrialization production and popularization and application, with realize " Laifeng County's Folium Crossostephii Chinensis " from
The simple transformation eaten raw with simple processed goods to high added value intensely processed products, improves " Laifeng County's Folium Crossostephii Chinensis " commodity
Value, drives " Laifeng County's Folium Crossostephii Chinensis " industrial chain extension and increases Planting household income, reduce field stockpiling of unsold product, increase
Plus agricultural performance, lift the higher value application level of local characteristic agricultural byproducts resource.Meanwhile, by " come
This provincial characteristics obvious distinguishing products are pushed to the whole nation, push the whole world to by the intensive processing product of phoenix Folium Crossostephii Chinensis ".
The content of the invention
The method that the technical problem to be solved in the present invention is to provide chlorogenic acid extracting in a kind of Folium Crossostephii Chinensis from Laifeng County.
The technical scheme is that：A kind of method of chlorogenic acid extracting in Folium Crossostephii Chinensis from Laifeng County, it is characterised in that bag
Include following steps：
A. digest
In extraction pot, Laifeng County's Folium Crossostephii Chinensis, water, cellulase, xylanase, B- glucanase and pectin are added
Enzyme；1-10 times for Laifeng County's Folium Crossostephii Chinensis weight of water addition, percentage ratio of the adjuvant addition for Laifeng County's Folium Crossostephii Chinensis weight：
Cellulase 0.1-1%, xylanase 0.1-1%, B- glucanase 0.3-3%, pectase 0.3-3%；Control
Hydrolysis temperature 35-55 degree, starts stirring, enzymolysis time：1-5 hours；
B. alcohol leaching
In extraction pot, 5-12 times of ethanol immersion of Laifeng County's Folium Crossostephii Chinensis weight, 2-24 hours are added；
C. microwave extraction
Control extraction pot temperature 50-95 degree, under the conditions of microwave power is 100-500kw, extracts 1-3 hours；
D. filter
Filtrate is obtained with 100-300 mesh sock filtrations, storage tank is preserved, and filtering residue is added 3-8 times of ethanol, carried again
Taking tank and extracting 2-6 hours, filtrate is obtained with 100-300 mesh sock filtrations, merging filtrate storage tank is preserved；
E. concentrate
Filtrate is stood after 6-24 hours, is concentrated into concentrator, temperature control in 60-70 degree, very
Reciprocal of duty cycle is concentrated in 0.8-0.95, is stopped when being more than 55% to material dry matter content；
F. cool down
Material is cooled to into room temperature, chlorogenic acid extractum of the solid matter relative content more than 55% is obtained.
The method of chlorogenic acid extracting in a kind of Folium Crossostephii Chinensis from Laifeng County of the present invention, it is characterised in that comprise the following steps：
A. digest
In extraction pot, Laifeng County's Folium Crossostephii Chinensis, water, cellulase, xylanase, B- glucanase and pectin are added
Enzyme；1-10 times for Laifeng County's Folium Crossostephii Chinensis weight of water addition, percentage ratio of the adjuvant addition for Laifeng County's Folium Crossostephii Chinensis weight：
Cellulase 0.1-1%, xylanase 0.1-1%, B- glucanase 0.3-3%, pectase 0.3-3%；Control
Hydrolysis temperature 35-55 degree, starts stirring, enzymolysis time：1-5 hours；
B. alcohol leaching
In extraction pot, 5-12 times of ethanol immersion of Laifeng County's Folium Crossostephii Chinensis weight, 2-24 hours are added；
C. microwave extraction
Control extraction pot temperature 50-95 degree, under the conditions of microwave power is 100-500kw, extracts 1-3 hours；
Microwave extraction system used：The maet-6 microwave extraction systems produced using Shanghai Jing Qiao drying equipments factory；
D. filter
Filtrate is obtained with 100-300 mesh sock filtrations, storage tank is preserved, and filtering residue is added 3-8 times of ethanol, carried again
Taking tank and extracting 2-6 hours, filtrate is obtained with 100-300 mesh sock filtrations, merging filtrate storage tank is preserved；
E. concentrate
Filtrate is stood after 6-24 hours, is concentrated into concentrator, temperature control in 60-70 degree, very
Reciprocal of duty cycle is concentrated in 0.8-0.95, reclaims ethanol first, ethanol is recovered to ethanol storage tank, when concentrated solution ethanol
Concentration meter is detected, during without ethanol, ethanol is reclaimed and stopped；Moisture evaporation is then proceeded by, to material dry
Matter content stops when being more than 55%；
F. cool down
Material is cooled to into room temperature, chlorogenic acid extractum of the solid matter relative content more than 55% is obtained.
The method of chlorogenic acid extracting in a kind of Folium Crossostephii Chinensis from Laifeng County of the present invention, Laifeng County's Folium Crossostephii Chinensis primary chemical used into
Point, research shows, in " Laifeng County's Folium Crossostephii Chinensis " main component have chlorogenic acid, luteolin, linarin, aminoacid,
The compositions such as polysaccharide, flavonoid, chlorogenic acid, volatile essential oil, determine the volatile ingredient of " Laifeng County's Folium Crossostephii Chinensis ",
And the general flavone content and volatile oil yield of the different Flos Chrysanthemis of comparison, as a result show, total flavones in " Laifeng County's Folium Crossostephii Chinensis "
Content and volatile oil content are higher, have cis-oxidation linalool (21.84%), spathulenol in volatile oil
(4.25%), her elemene (8.23%), her eudesmol (13.90%), have 2 in Static Headspace analysis,
3. butanediol (5.69%), only. phellandrene (31.05%), paracymene (38.08%), three. Lignum cinnamomi camphorae
Alcohol (7.63%), linalool oxide (29.38)；The basis of dry " Laifeng County's Folium Crossostephii Chinensis " is mainly：Dry
80%～90%, protein 1%～1.8%, carbohydrate 6.3%～10.8%, crude fibre 0.6%～1.7%,
Fat 0.1%, calcium 0.2～0.5%, phosphorus 0.05% and abundant vitamin A, B1, B2, C and micro
Ferrum, potassium, manganese, the mineral element such as zinc." Laifeng County's Folium Crossostephii Chinensis " are containing about 0.015% (dry product content is about 0.15%)
Ethereal oil, mainly aromatic, although content is seldom, it is distinctive that these compounds constitute which
Local flavor and physiological function composition, are one of focuses at present to the research of " Laifeng County's Folium Crossostephii Chinensis " physiologically active ingredient." come
Main function composition in phoenix Folium Crossostephii Chinensis " can be specifically divided into following a few classes:
Antioxidant activity.Chlorogenic acid and luteolin are the main components in " Laifeng County's Folium Crossostephii Chinensis ", oxidation resistance
Also it is stronger；Flavonoidss, are primarily present in leaf, stem and crust, with flavonoid, flavonols and
Anthocyan is representative；Phenylpropanoid glycoside, is primarily present in leaf, stem, including caffeic acid, Resina Ferulae
The monomers such as acid, sinapic acid and its derivant；Steroidal compounds and nitrogen-containing compound.
" Laifeng County's Folium Crossostephii Chinensis ", with its special Physiological Properties, " Laifeng County's Folium Crossostephii Chinensis " and " Laifeng County's Folium Crossostephii Chinensis " are deep
Converted productss have functions that bactericidal antiphlogistic, flat liver improving eyesight, dissipate wind blood pressure lowering, and Folium Crossostephii Chinensis are used to prevent and treat by Mountain Area of Western Hubei Province
The diseases such as flu, headache, bacillary dysentery, enteritis, constipation, coronary heart disease and hypertension.
The method of chlorogenic acid extracting in a kind of Folium Crossostephii Chinensis from Laifeng County of the present invention, process conditions require low, rational technology；
Extraction process is created, and is adapted to commercial production conditions, and extraction efficiency is high, while equipment is simple, low cost of manufacture,
Popularization and application are easy.
In the inventive method, raw material used, equipment are common common raw material, equipment, it is to avoid industrialization
For expensive raw materials, the dependence of instrument in production process, production cost is greatly reduced；Laifeng County's Folium Crossostephii Chinensis kind
Plant easy, cuttage, tissue culture, yield are high, moderate, and convenient sources, following resource are secure.Make
With Laifeng County's Folium Crossostephii Chinensis as raw material, the utilization ratio in Laifeng County's Folium Crossostephii Chinensis winter was both substantially increased, improved the attached of Laifeng County's Folium Crossostephii Chinensis
It is value added, broken away from for the dependence of the other materials such as raw material such as reseda, Semen arachidis hypogaeae shell again, market can have been alleviated
Wilderness demand to other raw materials, while and discarded Laifeng County's Folium Crossostephii Chinensis can be made full use of, protect reseda etc.
Plant resourceses.
The inventive method is simple to operate, it is not necessary to using resin chromatography filtering technique, it is not required that precision instrument or from
Dynamicization equipment, can be produced in the resourceful township enterprise of Laifeng County's Folium Crossostephii Chinensis, and this greatly reduces chlorogenic acid
Production cost, simplify production process.
Reagent used by the present invention is the chemical reagent of nontoxic, cheap, volume production, in whole process using into
The routine techniquess that ripe reagent is reclaimed, this greatly reduces to environmental emission garbage.
Specific embodiment
With reference to embodiment, the present invention is further described.
Embodiment 1：In a kind of Folium Crossostephii Chinensis from Laifeng County of the present invention, the method for chlorogenic acid extracting, comprises the following steps：
A. digest
In extraction pot, Laifeng County's Folium Crossostephii Chinensis, water, cellulase, xylanase, B- glucanase and pectin are added
Enzyme；1 times for Laifeng County's Folium Crossostephii Chinensis weight of water addition, percentage ratio of the adjuvant addition for Laifeng County's Folium Crossostephii Chinensis weight：It is fine
The plain enzyme 0.1% of dimension, xylanase 0.1%, B- glucanase 0.3%, pectase 0.3%；Controlled enzymatic hydrolysis temperature
35 degree, start stirring, enzymolysis time：1 hour；
B. alcohol leaching
In extraction pot, 5 times of ethanol of Laifeng County's Folium Crossostephii Chinensis weight are added to soak, 2 hours；
C. microwave extraction
50 degree of control extraction pot temperature, under the conditions of microwave power is 100kw, extracts 1 hour；Microwave used
Extraction system：The maet-6 microwave extraction systems produced using Shanghai Jing Qiao drying equipments factory；
D. filter
Filtrate is obtained with 100 mesh sock filtrations, storage tank is preserved, and filtering residue is added 3 times of ethanol, carried in extraction pot again
Taking 2 hours, filtrate being obtained with 100 mesh sock filtrations, merging filtrate storage tank is preserved；
E. concentrate
After filtrate is stood 6 hours, concentrated into concentrator, at 60 degree, vacuum exists temperature control
0.8 concentration, reclaims ethanol first, ethanol is recovered to ethanol storage tank, when concentrated solution is detected with ethanol concentration meter,
During without ethanol, ethanol is reclaimed and is stopped；Moisture evaporation is then proceeded by, is more than to material dry matter content
Stop when 55%；
F. cool down
Material is cooled to into room temperature, chlorogenic acid extractum of the solid matter relative content more than 55% is obtained.
Embodiment 2：In a kind of Folium Crossostephii Chinensis from Laifeng County of the present invention, the method for chlorogenic acid extracting, comprises the following steps：
A. digest
In extraction pot, Laifeng County's Folium Crossostephii Chinensis, water, cellulase, xylanase, B- glucanase and pectin are added
Enzyme；10 times for Laifeng County's Folium Crossostephii Chinensis weight of water addition, percentage ratio of the adjuvant addition for Laifeng County's Folium Crossostephii Chinensis weight：
Cellulase 1%, xylanase 1%, B- glucanase 3%, pectase 3%；55 degree of controlled enzymatic hydrolysis temperature,
Start stirring, enzymolysis time：5 hours；
B. alcohol leaching
In extraction pot, 12 times of ethanol of Laifeng County's Folium Crossostephii Chinensis weight are added to soak, 24 hours；
C. microwave extraction
95 degree of control extraction pot temperature, under the conditions of microwave power is 500kw, extracts 3 hours；Microwave used
Extraction system：The maet-6 microwave extraction systems produced using Shanghai Jing Qiao drying equipments factory；
D. filter
Filtrate is obtained with 300 mesh sock filtrations, storage tank is preserved, and filtering residue is added 8 times of ethanol, carried in extraction pot again
Taking 6 hours, filtrate being obtained with 300 mesh sock filtrations, merging filtrate storage tank is preserved；
E. concentrate
After filtrate is stood 24 hours, concentrated into concentrator, at 70 degree, vacuum exists temperature control
0.95 concentration, reclaims ethanol first, ethanol is recovered to ethanol storage tank, when concentrated solution is detected with ethanol concentration meter,
During without ethanol, ethanol is reclaimed and is stopped；Moisture evaporation is then proceeded by, is more than to material dry matter content
Stop when 55%；
F. cool down
Material is cooled to into room temperature, chlorogenic acid extractum of the solid matter relative content more than 55% is obtained.
Embodiment 3：In a kind of Folium Crossostephii Chinensis from Laifeng County of the present invention, the method for chlorogenic acid extracting, comprises the following steps：
A. digest
In extraction pot, Laifeng County's Folium Crossostephii Chinensis, water, cellulase, xylanase, B- glucanase and pectin are added
Enzyme；5 times for Laifeng County's Folium Crossostephii Chinensis weight of water addition, percentage ratio of the adjuvant addition for Laifeng County's Folium Crossostephii Chinensis weight：It is fine
The plain enzyme 0.5% of dimension, xylanase 0.5%, B- glucanase 1.5%, pectase 1.5%；Controlled enzymatic hydrolysis temperature
45 degree, start stirring, enzymolysis time：2.5 hour；
B. alcohol leaching
In extraction pot, 8 times of ethanol of Laifeng County's Folium Crossostephii Chinensis weight are added to soak, 12 hours；
C. microwave extraction
75 degree of control extraction pot temperature, under the conditions of microwave power is 300kw, extracts 1.5 hours；It is used micro-
Ripple extraction system：The maet-6 microwave extraction systems produced using Shanghai Jing Qiao drying equipments factory；
D. filter
Filtrate is obtained with 200 mesh sock filtrations, storage tank is preserved, and filtering residue adds 5.5 times of ethanol, again in extraction pot
Extracting 4 hours, filtrate being obtained with 200 mesh sock filtrations, merging filtrate storage tank is preserved；
E. concentrate
After filtrate is stood 15 hours, concentrated into concentrator, at 65 degree, vacuum exists temperature control
0.9 concentration, reclaims ethanol first, ethanol is recovered to ethanol storage tank, when concentrated solution is detected with ethanol concentration meter,
During without ethanol, ethanol is reclaimed and is stopped；Moisture evaporation is then proceeded by, is more than to material dry matter content
Stop when 55%；
F. cool down
Material is cooled to into room temperature, chlorogenic acid extractum of the solid matter relative content more than 55% is obtained.
Embodiment 4：In a kind of Folium Crossostephii Chinensis from Laifeng County of the present invention, the method for chlorogenic acid extracting, comprises the following steps：
A. digest
In extraction pot, Laifeng County's Folium Crossostephii Chinensis, water, cellulase, xylanase, B- glucanase and pectin are added
Enzyme；8 times for Laifeng County's Folium Crossostephii Chinensis weight of water addition, percentage ratio of the adjuvant addition for Laifeng County's Folium Crossostephii Chinensis weight：It is fine
The plain enzyme 0.8% of dimension, xylanase 0.8%, B- glucanase 2%, pectase 2%；Controlled enzymatic hydrolysis temperature 50
Degree, starts stirring, enzymolysis time：4 hours；
B. alcohol leaching
In extraction pot, 10 times of ethanol of Laifeng County's Folium Crossostephii Chinensis weight are added to soak, 20 hours；
C. microwave extraction
80 degree of control extraction pot temperature, under the conditions of microwave power is 400kw, extracts 2 hours；Microwave used
Extraction system：The maet-6 microwave extraction systems produced using Shanghai Jing Qiao drying equipments factory；
D. filter
Filtrate is obtained with 250 mesh sock filtrations, storage tank is preserved, and filtering residue is added 7 times of ethanol, carried in extraction pot again
Taking 5 hours, filtrate being obtained with 250 mesh sock filtrations, merging filtrate storage tank is preserved；
E. concentrate
After filtrate is stood 20 hours, concentrated into concentrator, at 68 degree, vacuum exists temperature control
0.92 concentration, reclaims ethanol first, ethanol is recovered to ethanol storage tank, when concentrated solution is detected with ethanol concentration meter,
During without ethanol, ethanol is reclaimed and is stopped；Moisture evaporation is then proceeded by, is more than to material dry matter content
Stop when 55%；
F. cool down
Material is cooled to into room temperature, chlorogenic acid extractum of the solid matter relative content more than 55% is obtained.
Embodiment 5：In a kind of Folium Crossostephii Chinensis from Laifeng County of the present invention, the method for chlorogenic acid extracting, comprises the following steps：
A. digest
In extraction pot, Laifeng County's Folium Crossostephii Chinensis, water, cellulase, xylanase, B- glucanase and pectin are added
Enzyme；4 times for Laifeng County's Folium Crossostephii Chinensis weight of water addition, percentage ratio of the adjuvant addition for Laifeng County's Folium Crossostephii Chinensis weight：It is fine
The plain enzyme 0.4% of dimension, xylanase 0.4%, B- glucanase 1%, pectase 1%；Controlled enzymatic hydrolysis temperature 38
Degree, starts stirring, enzymolysis time：2 hours；
B. alcohol leaching
In extraction pot, 8 times of ethanol of Laifeng County's Folium Crossostephii Chinensis weight are added to soak, 5 hours；
C. microwave extraction
70 degree of control extraction pot temperature, under the conditions of microwave power is 150kw, extracts 1.2 hours；It is used micro-
Ripple extraction system：The maet-6 microwave extraction systems produced using Shanghai Jing Qiao drying equipments factory；
D. filter
Filtrate is obtained with 150 mesh sock filtrations, storage tank is preserved, and filtering residue is added 4 times of ethanol, carried in extraction pot again
Taking 3 hours, filtrate being obtained with 150 mesh sock filtrations, merging filtrate storage tank is preserved；
E. concentrate
After filtrate is stood 8 hours, concentrated into concentrator, at 68 degree, vacuum exists temperature control
0.85 concentration, reclaims ethanol first, ethanol is recovered to ethanol storage tank, when concentrated solution is detected with ethanol concentration meter,
During without ethanol, ethanol is reclaimed and is stopped；Moisture evaporation is then proceeded by, is more than to material dry matter content
Stop when 55%；
F. cool down
Material is cooled to into room temperature, chlorogenic acid extractum of the solid matter relative content more than 55% is obtained.
Embodiment 6：In a kind of Folium Crossostephii Chinensis from Laifeng County of the present invention, the method for chlorogenic acid extracting, comprises the following steps：
A. digest
In extraction pot, Laifeng County's Folium Crossostephii Chinensis, water, cellulase, xylanase, B- glucanase and pectin are added
Enzyme；6 times for Laifeng County's Folium Crossostephii Chinensis weight of water addition, percentage ratio of the adjuvant addition for Laifeng County's Folium Crossostephii Chinensis weight：It is fine
The plain enzyme 0.6% of dimension, xylanase 0.6%, B- glucanase 2.1%, pectase 2.1%；Controlled enzymatic hydrolysis temperature
39 degree, start stirring, enzymolysis time：4 hours；
B. alcohol leaching
In extraction pot, 7 times of ethanol of Laifeng County's Folium Crossostephii Chinensis weight are added to soak, 20 hours；
C. microwave extraction
80 degree of control extraction pot temperature, under the conditions of microwave power is 400kw, extracts 2.5 hours；It is used micro-
Ripple extraction system：The maet-6 microwave extraction systems produced using Shanghai Jing Qiao drying equipments factory；
D. filter
Filtrate is obtained with 300 mesh sock filtrations, storage tank is preserved, and filtering residue is added 6 times of ethanol, carried in extraction pot again
Taking 5 hours, filtrate being obtained with 300 mesh sock filtrations, merging filtrate storage tank is preserved；
E. concentrate
After filtrate is stood 22 hours, concentrated into concentrator, at 66 degree, vacuum exists temperature control
0.89 concentration, reclaims ethanol first, ethanol is recovered to ethanol storage tank, when concentrated solution is detected with ethanol concentration meter,
During without ethanol, ethanol is reclaimed and is stopped；Moisture evaporation is then proceeded by, is more than to material dry matter content
Stop when 55%；
F. cool down
Material is cooled to into room temperature, chlorogenic acid extractum of the solid matter relative content more than 55% is obtained.
Claims (2)
1. in a kind of Folium Crossostephii Chinensis from Laifeng County chlorogenic acid extracting method, it is characterised in that comprise the following steps：
A. digest
In extraction pot, Laifeng County's Folium Crossostephii Chinensis, water, cellulase, xylanase, B- glucanase and pectin are added
Enzyme；1-10 times for Laifeng County's Folium Crossostephii Chinensis weight of water addition, percentage ratio of the adjuvant addition for Laifeng County's Folium Crossostephii Chinensis weight：
Cellulase 0.1-1%, xylanase 0.1-1%, B- glucanase 0.3-3%, pectase 0.3-3%；Control
Hydrolysis temperature 35-55 degree, starts stirring, enzymolysis time：1-5 hours；
B. alcohol leaching
In extraction pot, 5-12 times of ethanol immersion of Laifeng County's Folium Crossostephii Chinensis weight, 2-24 hours are added；
C. microwave extraction
Control extraction pot temperature 50-95 degree, under the conditions of microwave power is 100-500kw, extracts 1-3 hours；
D. filter
Filtrate is obtained with 100-300 mesh sock filtrations, storage tank is preserved, and filtering residue is added 3-8 times of ethanol, carried again
Taking tank and extracting 2-6 hours, filtrate is obtained with 100-300 mesh sock filtrations, merging filtrate storage tank is preserved；
E. concentrate
Filtrate is stood after 6-24 hours, is concentrated into concentrator, temperature control in 60-70 degree, very
Reciprocal of duty cycle is concentrated in 0.8-0.95, is stopped when being more than 55% to material dry matter content；
F. cool down
Material is cooled to into room temperature, chlorogenic acid extractum of the solid matter relative content more than 55% is obtained.
2. according to the method for chlorogenic acid extracting in a kind of Folium Crossostephii Chinensis from Laifeng County described in claim 1, it is characterised in that
Comprise the following steps：
A. digest
In extraction pot, Laifeng County's Folium Crossostephii Chinensis, water, cellulase, xylanase, B- glucanase and pectin are added
Enzyme；1-10 times for Laifeng County's Folium Crossostephii Chinensis weight of water addition, percentage ratio of the adjuvant addition for Laifeng County's Folium Crossostephii Chinensis weight：
Cellulase 0.1-1%, xylanase 0.1-1%, B- glucanase 0.3-3%, pectase 0.3-3%；Control
Hydrolysis temperature 35-55 degree, starts stirring, enzymolysis time：1-5 hours；
B. alcohol leaching
In extraction pot, 5-12 times of ethanol immersion of Laifeng County's Folium Crossostephii Chinensis weight, 2-24 hours are added；
C. microwave extraction
Control extraction pot temperature 50-95 degree, under the conditions of microwave power is 100-500kw, extracts 1-3 hours；
Microwave extraction system used：The maet-6 microwave extraction systems produced using Shanghai Jing Qiao drying equipments factory；
D. filter
Filtrate is obtained with 100-300 mesh sock filtrations, storage tank is preserved, and filtering residue is added 3-8 times of ethanol, carried again
Taking tank and extracting 2-6 hours, filtrate is obtained with 100-300 mesh sock filtrations, merging filtrate storage tank is preserved；
E. concentrate
Filtrate is stood after 6-24 hours, is concentrated into concentrator, temperature control in 60-70 degree, very
Reciprocal of duty cycle is concentrated in 0.8-0.95, reclaims ethanol first, ethanol is recovered to ethanol storage tank, when concentrated solution ethanol
Concentration meter is detected, during without ethanol, ethanol is reclaimed and stopped；Moisture evaporation is then proceeded by, to material dry
Matter content stops when being more than 55%；
F. cool down
Material is cooled to into room temperature, chlorogenic acid extractum of the solid matter relative content more than 55% is obtained.
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