CN106832045B - A kind of method that gingko episperm extracts pectin and phenolic acid compound simultaneously - Google Patents
A kind of method that gingko episperm extracts pectin and phenolic acid compound simultaneously Download PDFInfo
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- CN106832045B CN106832045B CN201510870230.8A CN201510870230A CN106832045B CN 106832045 B CN106832045 B CN 106832045B CN 201510870230 A CN201510870230 A CN 201510870230A CN 106832045 B CN106832045 B CN 106832045B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0045—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Galacturonans, e.g. methyl ester of (alpha-1,4)-linked D-galacturonic acid units, i.e. pectin, or hydrolysis product of methyl ester of alpha-1,4-linked D-galacturonic acid units, i.e. pectinic acid; Derivatives thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/06—Coniferophyta [gymnosperms], e.g. cypress
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/16—Ginkgophyta, e.g. Ginkgoaceae (Ginkgo family)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/35—Extraction with lipophilic solvents, e.g. Hexane or petrol ether
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/10—General cosmetic use
Abstract
The invention discloses a kind of methods for extracting pectin and phenolic acid compound simultaneously from gingko episperm, are characterized in that: (1) selection picks ginkgo in the Chinese olive phase；(2) gingko episperm is smashed to pieces after rinsing using food masher；(3) gingko episperm smashed to pieces leaches in leaching liquid；(4) the pectin solution activity carbon decoloring that leaching obtains；(5) pectin solution after decolourizing is concentrated using ceramic super-filtering film；(6) pectin solution after being concentrated uses ethanol precipitation；(7) pectin crude extract is purified using ethyl alcohol immersion process；(8) pectin drying after purification, is ground into pectin powder.(9) filter residue obtained after pectin extraction extracts ginkgolic acid using ethanol solution；(10) phenolic acid crude extract carries out reextraction with petroleum ether, and extract liquor carries out chromatography using large pore resin absorption column, is dried in vacuo after ethanol gradient elution, obtains faint yellow ginkgolic acid extract.
Description
Technical field
This technology is related to food and medicine field, and in particular to one kind extracts pectin and phenolic acid class simultaneously from gingko episperm
The method of compound.
Background technique
Ginkgo is Ginkgoaceae ginkgo platymiscium also known as Gong Sunshu, maidenhair tree, is the distinctive precious medicinal plant in China,
Leaf, fruit and exosper etc. all have medicinal Development volue, referred to as " whole body is all precious living fossil ".Made of being developed as ginkgo leaf
Ginkgo biloba extract preparation is well received one of natural drug, and various nutraceutical made of being developed as gingko are also very much, only
There is the utilization rate of gingko episperm lower.According to statistics, there are about 30,000 tons or so exospers every year in China is lost as waste
It abandons, is not exploited, not only waste of resource but also polluted environment, and skin contact can also cause to paint malicious sample dermatitis.There is research to send out
Existing gingko episperm has many-sided pharmacological activity, has higher utility value, can be used for drug, health care product and plant pesticide
Exploitation, has broad application prospects.Therefore, study, develop gingko episperm biological products to comprehensive utilization gingko resource and
It preserves the ecological environment and is of great significance, it has also become the hot subject of current research.Gingko episperm is the cortex of food containing gingko almond,
That is seed hard shell exterior portion, is commonly called as gingko afterbirth, and quality accounts for the 70% of entire seed.Gingko episperm complicated component, contains
There are many active chemical components and nutritional ingredient, wherein pectin and ginkgolic acid are the higher ingredients of content, in gingko episperm
Pectin content can reach the 13% of ginkgo nut total weight, and the content of phenolic acid is 3.54%.Pectin is a kind of natural polysaccharide
High molecular polymer is white to yellowish-brown powder, has colorless and odorless, without the properties such as definite melting point and solubility, does not dissolve in
The organic solvents such as ethyl alcohol, but it is dissolved in hot water, it is slightly soluble in cold water.Pectin be the seventh-largest nutrient diet fiber of human body it is main at
Point, there is multiple eating and medical value, had a wide range of applications in food, medicine and other fields.In gingko episperm containing compared with
High phenolic acid can be divided into ginkgolic acid, hydroginkgoic acid, hydroginkgolinic acid, bilobol, silver by the difference of chemical structure
16 kinds of apricot phenol etc. or more.Research shows that ginkgolic acid has antitumor, anti-inflammatory, antiallergy, antibacterial, prevention and treatment pest and disease damage and other effects,
There is good application value in terms of food, cosmetics, biological pesticide and medicine.
Traditional pectin extraction method has boiling water extraction process, acid hydrolyzation, microbial method, microwave―assisted extraction etc., industry
Acid extraction method is generallyd use in production, this method is low with production equipment requirement, technique is more simple and easy to control, is easy to amplify, obtain
The advantages that pectin arrived is high-quality, with high purity.But also have the shortcomings that energy consumption is high, consumption of organic solvent is big, processing wastewater flow rate is big.
Separating Ginkgo phenolic acids compound extracting method mainly uses the lower organic solvent extraction of n-hexane, chloroform, ether isopolarity, although
The impurity of dissolution is few, but the permeability of solvent is not strong, and consumption is big, and toxicity is also big, higher cost.The extraction side of ginkgo product at present
Method only extracts single substance, such as acidity extraction pectin only obtains water-soluble preferable pectin product, the water solubilitys such as phenolic acid
Poor compound is taken as impurity treatment and falls, this not only wastes resource and also increases the difficulty of waste water, Solid state fermentation, simultaneously
Solvent utilization rate and production efficiency is not also high.Therefore, it is necessary to develop good separating effect, extraction efficiency are high, solvent utilization rate is high,
Cost is relatively low, extracts pectin and phenolic acid compound new process in slave gingko episperm with industrialized production future simultaneously
And new method.
Summary of the invention
The purpose of the present invention is exploitation good separating effect, extraction efficiency is high, solvent utilization rate is high, cost is relatively low, has
Pectin and phenolic acid compound new method are extracted in the slave gingko episperm of industrialized production future simultaneously.
That the purpose of the present invention is development qualities is high, extraction efficiency is high, can be with the gingko episperm fruit of industrialized production
Glue new method for extracting.
Definition: gingko episperm: ginkgo is gymnosperm, is wrapped in gingko seed (gingko seed includes pulp and shell)
The part of outer similar pulp is exosper.
1, a kind of gingko episperm pectin extraction and compound of phenolic acid method, which is characterized in that in turn include the following steps:
(1) picking of ginkgo fruit
Selection picks ginkgo in Chinese olive phase (the 7-9 month), and it is spare to strip exosper；
(2) gingko episperm pre-processes
Gingko episperm first pass around screening removal go rotten, corruption raw material, it is selected after starting material with water rinse 2-5 times,
Wind drenches 5-30min, is then crushed gingko episperm using food masher；
(3) pectin leaches
The ratio of 1:5-1:30 adds leaching liquid, leaching liquid solute composition into the gingko episperm of crushing in mass ratio
Are as follows: sodium phosphate (Na3PO4) 2-8wt%, disodium hydrogen phosphate (Na2HPO4) 0.5-4wt%, sodium citrate (Na3C6H5O7)10-
100mM, hydroxyacetic acid (HOCH2COOH) 0.2-1wt%；Leaching liquid salt acid for adjusting pH value to 2-6；It is stirred at 70-90 DEG C
Leach 45-120min；Leaching operation reactor is 3-8 fixed bed reactors, using multi-stage batch counter-current extraction operating procedure
(counter-current extraction process refers to that material and leaching liquid are flowed at opposite direction, and material is from left side reactor reactor stream to the right
Dynamic, leaching liquid is from right side reactor reactor flow to the left)；It is molten using plate filter filtering acquisition pectin after leaching
Liquid；
(4) pectin solution decolourizes
Active carbon, and the 30- that decolourizes under the conditions of 50-70 DEG C of temperature are added in step (3) filtered pectin solution
The ratio of 120min, pectin solution and active carbon is 1L:5-20g；Filtering obtains pectin solution；
(5) pectin solution is concentrated
Step (4) filtered pectin solution is cooled to room temperature, and is concentrated using ceramic super-filtering film, solution body after concentration
Product is the 20-50% that preceding original solution volume is concentrated, and ultrafiltration retaining molecular weight is 10,000-300,000, and operating pressure is
0.05-0.3MPa, operation temperature are room temperature；Obtain fructose concentrating liquid；
(6) pectin ethanol precipitation
The ethanol water of volumetric concentration 85-95% is added in step (5) fructose concentrating liquid, controls ethyl alcohol in mixed liquor
Final volume concentration is 50%-80%, is stirred evenly, and adjusts the pH value of mixed liquor to 3-6, standing 0.5-4 hours to be precipitated complete
After filter, solid matter be obtain pectin crude extract；
(7) pectin crude extract purifies
The pectin crude extract that step (6) obtains is purified using ethyl alcohol immersion process, and concentration of alcohol is followed successively by dehydrated alcohol, body
Product concentration 88-92% ethanol water and volumetric concentration 78-82% ethanol water, soaking temperature are room temperature, when every section of immersion
Between be 30-90min；
(8) pectin is dry
Pectin after purification is dried at 50-70 DEG C, is then comminuted into pectin powder.
(9) ginkgolic acid leaches
The filter residue that step (3) is obtained by filtration is that leaching agent is leached with ethyl alcohol, and leaching carries out 3 times altogether, and the 1st leaching is adopted
Use ethanol solution collected by step (6) as leaching liquid carry out, ethyl alcohol volumetric concentration be 60-80%, solid-liquid ratio 1:5-15,
Reflux temperature is 50-70 DEG C, extraction time 30-240min；2nd leaching is made using ethanol solution collected by step (7)
For leaching liquid progress, ethyl alcohol volumetric concentration is 60-80%, and solid-liquid ratio 1:5-15, reflux temperature is 50-70 DEG C, extraction time
For 30-240min；3rd leaching is carried out using the ethanol solution of volumetric concentration 60-80%, solid-liquid ratio 1:5-15, reflux temperature
Degree is 50-70 DEG C, extraction time 30-240min；It collects leaching liquid and is filtered with plate and frame filter press, vacuum distillation obtains ginkgo
Phenolic acid crude extract.
(10) ginkgolic acid separates
The ginkgolic acid crude extract that step (9) obtains carries out reextraction with petroleum ether, after standing 60-240min, collects
Extract liquor carries out chromatography with 101 type large pore resin absorption columns, uses concentration to use volumetric concentration for 45-55%, 65-
75%, the ethanol solution of 85-95% carries out gradient elution, and eluting temperature is 25-55 DEG C, and eluent is laggard through vacuum distillation concentration
Row vacuum drying, obtains faint yellow ginkgolic acid extract.
Above-mentioned gingko episperm pectin and ginkgolic acid extraction method, step (1) are as follows: select the Chinese olive in ginkgo
Phase (the 7-9 month) picking, is placed in ventilated environment storage, spare, and when processing strips exosper；
Further, above-mentioned gingko episperm pectin and ginkgolic acid extraction method, step (2) are as follows: outside ginkgo
Kind of skin first pass around screening removal go rotten, the raw material of corruption, it is selected after raw material rinse 3 times, wind drenches 10min, then using food
Product pulverizer crushes gingko episperm；
Further, above-mentioned gingko episperm pectin and ginkgolic acid extraction method, step (3) are as follows: press quality
Ratio than 1:5-1:30 adds leaching liquid, leaching liquid composition: sodium phosphate (Na3PO4) 2- into the gingko episperm of crushing
8%, disodium hydrogen phosphate (Na2HPO4) 0.5-4%, sodium citrate (Na3C6H5O7) 10-100mM, hydroxyacetic acid
(HOCH2COOH) 0.2-1%.Leaching operation reactor is 3-8 fixed bed reactors, is operated using multi-stage batch counter-current extraction
(counter-current extraction process refers to that material and leaching liquid are flowed at opposite direction to technique, and material is from left side reactor side reaction to the right
Device flowing, leaching liquid is from right side reactor reactor flow to the left)；
Further, above-mentioned gingko episperm pectin and ginkgolic acid extraction method, step (4) are as follows: pectin is molten
Liquid is using active carbon decoloring, and 50-70 DEG C of bleaching temperature, bleaching time 30-120min, the ratio of pectin solution and active carbon is
1L:5-20g；
Further, above-mentioned gingko episperm pectin and ginkgolic acid extraction method, step (5) are as follows: using pottery
Pectin solution is concentrated in porcelain ultrafiltration membrane, and volume is the 20-50% of original solution volume after concentration, and ultrafiltration retaining molecular weight is 10,
000-300,000, operating pressure 0.05-0.3Mpa；
Further, above-mentioned gingko episperm pectin and ginkgolic acid extraction method, step (6) are as follows: pectin is dense
Contracting liquid uses ethanol precipitation pectin, and the final volume concentration of ethyl alcohol is 50%-80%, and the pH of solution is 3-6, time of repose 0.5-
4 hours；
Further, above-mentioned gingko episperm pectin and ginkgolic acid extraction method, step (7) are as follows: pectin is thick
Extract is purified using ethyl alcohol immersion process, removes small molecule and oil-soluble impurities, it is dense that concentration of alcohol is followed successively by dehydrated alcohol, volume
It spends 88-92% ethanol water and volumetric concentration 78-82% ethanol water, soaking temperature is room temperature, soaking time 30-
90min；
Further, above-mentioned gingko episperm pectin and ginkgolic acid extraction method, step (8) are as follows: after purification
Pectin dried at 50-70 DEG C, be then comminuted into pectin powder.
Further, above-mentioned gingko episperm pectin and ginkgolic acid extraction method, step (9) are as follows: step (3)
The filter residue being obtained by filtration is that leaching agent is leached with ethyl alcohol, and leaching carries out 3 times altogether, the 1st leaching is received using step (6)
The ethanol solution of collection is carried out as leaching liquid, and ethyl alcohol volumetric concentration is 60-80%, solid-liquid ratio 1:5-15, reflux temperature 50-
70 DEG C, extraction time 30-240min；2nd leaching is carried out using ethanol solution collected by step (7) as leaching liquid,
Ethyl alcohol volumetric concentration is 60-80%, and solid-liquid ratio 1:5-15, reflux temperature is 50-70 DEG C, extraction time 30-240min；The
3 leachings are carried out using the ethanol solution of volumetric concentration 60-80%, solid-liquid ratio 1:5-15, and reflux temperature is 50-70 DEG C, are mentioned
Taking the time is 30-240min；It collects leaching liquid and is filtered with plate and frame filter press, vacuum distillation obtains ginkgolic acid crude extract.
Further, above-mentioned gingko episperm pectin and ginkgolic acid extraction method, step (10) are as follows: step
(9) the ginkgolic acid crude extract obtained carries out reextraction with petroleum ether, after standing 60-240min, collects 101 types of extract liquor
Large pore resin absorption column carries out chromatography, uses concentration to use volumetric concentration for 45-55%, 65-75%, 85-95%
Ethanol solution carries out gradient elution, and eluting temperature is 25-55 DEG C, and eluent is dried in vacuo after vacuum distillation concentration, obtains
To faint yellow ginkgolic acid extract.
Compared with prior art, technical solution provided by the invention has following technological merit:
(1) the characteristics of present invention chooses the Chinese olive phase (the 7-9 month) that gingko episperm is fruit, which picks is that pectin contains
Amount is high, easily stored and progress pre-treatment.
(2) technical solution provided by the invention has prepared a kind of new gingko episperm pectin leaching liquid, and fruit can be improved
Glue extraction efficiency.
(3) technical solution pectin leaching provided by the invention leaches operating procedure using multi-stage countercurrent, and pectin can be improved
Extraction efficiency, while the dosage of leaching liquid can also be reduced, reduce production cost.
(4) technical solution pectin crude extract provided by the invention is purified using ethyl alcohol immersion process, removes small molecule and rouge
Solubility impurity can be improved the quality of pectin, and can reduce ethanol consumption using multistage dip operation technique, reduce energy
Consumption.
(5) technical solution provided by the invention can extract pectin and ginkgolic acid simultaneously in gingko episperm, improve
The utilization rate of gingko resource.
(6) technical solution provided by the invention provides a kind of production technology for comprehensively utilizing pectin purification solvent, can be with
Solvent utilization rate is improved, solvent usage amount is reduced.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but do not constitute any limitation of the invention.Anyone is within the scope of the invention as claimed
Any type of modification made, still within the claims in the present invention protection scope.
Embodiment 1
The method that a kind of gingko episperm provided by the invention extracts pectin and phenolic acid compound simultaneously successively includes such as
Lower step:
(1) picking of ginkgo fruit
It selects to pick in the Chinese olive phase (the 7-9 month) of ginkgo, is placed in ventilated environment and stores；It is spare to strip exosper.
(2) gingko episperm pre-processes
Weigh 1000 grams of gingko episperms, by screening removal go rotten, corruption raw material, will be selected after raw material rinse 3
There may be the impurity such as soil, sandstone, iron filings, wind to drench 10min, be crushed raw material using food masher for secondary removal.
(3) pectin leaches
The ratio of 1:10 adds leaching liquid, leaching liquid composition are as follows: sodium phosphate into the raw material of crushing in mass ratio
(Na3PO4) 3%, disodium hydrogen phosphate (Na2HPO4) 0.9%, sodium citrate (Na3C6H5O7) 50mM, hydroxyacetic acid
(HOCH2COOH) 0.4%.PH value is adjusted to 2 with hydrochloric acid (HCl), stirs 90min at 80 DEG C.Leaching operation reactor is 3
Fixed bed reactors, using multi-stage batch counter-current extraction operating procedure；Fruit is obtained using plate filter filtering after leaching
Sol solution.
(4) pectin solution decolourizes
Addition active carbon in pectin solution after filtration, and the 60min that decolourizes at 50 DEG C, pectin solution and active carbon
Ratio is 1L:15g.It is filtered after decoloration using plate filter.
(5) pectin solution is concentrated
Filtered pectin solution is cooled to room temperature, and is concentrated using ceramic super-filtering film, and liquor capacity is original after concentration
The 30% of liquor capacity, ultrafiltration retaining molecular weight are 300,000, and operating pressure 0.1MPa, operation temperature is room temperature.
(6) pectin ethanol precipitation
95% ethanol solution is added in pectin solution after concentration, controls final concentration of 70% of ethyl alcohol in mixed liquor,
It stirs evenly, the pH value for adjusting mixed liquor with hydrochloric acid (HCl) stands completely rear filtering to be precipitated in 4 hours, obtain pectin to 3.5
Crude extract.
(7) pectin crude extract purifies
Pectin crude extract is purified using ethyl alcohol immersion process, removes small molecule and oil-soluble impurities, concentration of alcohol are followed successively by
Dehydrated alcohol, 90% and 80%, soaking temperature are room temperature, and every section of soaking time is 45min.
(8) pectin is dry
Pectin after purification is dried at 55 DEG C, is then comminuted into pectin powder.
(9) ginkgolic acid leaches
It is that leaching agent is leached that the filter residue obtained after pectin, which is extracted, with ethyl alcohol, and leaching carries out 3 times altogether, and the 1st time using step
Suddenly ethanol solution collected by (6) is carried out as leaching liquid, and ethyl alcohol volumetric concentration is 70%, solid-liquid ratio 1:5, and reflux temperature is
60 DEG C, extraction time 60min；2nd leaching is carried out using ethanol solution collected by step (7) as leaching liquid, ethyl alcohol
Volumetric concentration is 85%, solid-liquid ratio 1:5, and reflux temperature is 60 DEG C, extraction time 60min；3rd leaching is dense using volume
The ethanol solution of degree 95% carries out, solid-liquid ratio 1:5, and reflux temperature is 60 DEG C, extraction time 120min；Collect leaching liquid simultaneously
It is filtered with plate and frame filter press, vacuum distillation obtains ginkgolic acid crude extract.
(10) ginkgolic acid separates
The ginkgolic acid crude extract that step (9) obtains carries out reextraction with petroleum ether, after standing 60min, collects extraction
Liquid carries out chromatography with 101 type large pore resin absorption columns, and volumetric concentration is used to carry out for 50,70%, 90% ethanol solution
Gradient elution, eluting temperature are 30 DEG C, and eluent is dried in vacuo after vacuum distillation concentration, obtain faint yellow ginkgolic acid
Extract.
(11) it calculates recovery rate: obtaining 130 grams of jelly powders, calculate 130 grams/1000 grams of recovery rate, obtaining recovery rate is
13%；32 grams of ginkgolic acids are obtained, calculate 32 grams/1000 grams of recovery rate, obtaining recovery rate is 3.2%.
The comparative example 1:(maturity period picks the gingko episperm of fruit, extracts pectin experiment)
(1) picking of ginkgo fruit
Maturity period (fruit yellow, matter is soft, mature) picking in ginkgo is selected, is placed in ventilated environment and stores, strip
Exosper is spare.
(2) gingko episperm pre-processes
Weigh 1000 grams of gingko episperms, by screening removal go rotten, corruption raw material, will be selected after raw material rinse 3
There may be the impurity such as soil, sandstone, iron filings, wind to drench 10min, be crushed raw material using food masher for secondary removal.
(3) pectin leaches
The ratio of 1:10 adds leaching liquid, leaching liquid composition are as follows: sodium phosphate into the raw material of crushing in mass ratio
(Na3PO4) 3%, disodium hydrogen phosphate (Na2HPO4) 0.9%, sodium citrate (Na3C6H5O7) 50mM, hydroxyacetic acid
(HOCH2COOH) 0.4%.PH value is adjusted to 2 with hydrochloric acid (HCl), stirs 90min at 80 DEG C.Leaching operation reactor is 3
Fixed bed reactors, using multi-stage batch counter-current extraction operating procedure；Fruit is obtained using plate filter filtering after leaching
Sol solution.
(4) pectin solution decolourizes
Addition active carbon in pectin solution after filtration, and the 60min that decolourizes at 50 DEG C, pectin solution and active carbon
Ratio is 1L:15g.It is filtered after decoloration using plate filter.
(5) pectin solution is concentrated
Filtered pectin solution is cooled to room temperature, and is concentrated using ceramic super-filtering film, and liquor capacity is original after molten contracting
The 30% of liquor capacity, ultrafiltration retaining molecular weight are 300,000, and operating pressure 0.1MPa, operation temperature is room temperature.
(6) pectin ethanol precipitation
95% ethanol solution is added in pectin solution after concentration, controls final concentration of 70% of ethyl alcohol in mixed liquor,
It stirs evenly, adjusts the pH value of mixed liquor to 3.5, stand completely rear filtering to be precipitated in 4 hours, obtain pectin crude extract.
(7) pectin crude extract purifies
Pectin crude extract is purified using ethyl alcohol immersion process, removes small molecule and oil-soluble impurities, concentration of alcohol are followed successively by
Dehydrated alcohol, 90% and 80%, soaking temperature are room temperature, soaking time 45min.
(8) pectin is dry
Pectin after purification is dried at 55 DEG C, is then comminuted into pectin powder.
(9) ginkgolic acid leaches
It is that leaching agent is leached that the filter residue obtained after pectin, which is extracted, with ethyl alcohol, and leaching carries out 3 times altogether, and the 1st time using step
Suddenly ethanol solution collected by (6) is carried out as leaching liquid, and ethyl alcohol volumetric concentration is 70%, solid-liquid ratio 1:5, and reflux temperature is
60 DEG C, extraction time 60min；2nd leaching is carried out using ethanol solution collected by step (7) as leaching liquid, ethyl alcohol
Volumetric concentration is 85%, solid-liquid ratio 1:5, and reflux temperature is 60 DEG C, extraction time 60min；3rd leaching is dense using volume
The ethanol solution of degree 95% carries out, solid-liquid ratio 1:5, and reflux temperature is 60 DEG C, extraction time 120min；Collect leaching liquid simultaneously
It is filtered with plate and frame filter press, vacuum distillation obtains ginkgolic acid crude extract.
(10) ginkgolic acid separates
The ginkgolic acid crude extract that step (9) obtains carries out reextraction with petroleum ether, after standing 60min, collects extraction
Liquid carries out chromatography with 101 type large pore resin absorption columns, and volumetric concentration is used to carry out for 50,70%, 90% ethanol solution
Gradient elution, eluting temperature are 30 DEG C, and eluent is dried in vacuo after vacuum distillation concentration, obtain faint yellow ginkgolic acid
Extract.
(11) it calculates recovery rate: obtaining 80 grams of jelly powders.80 grams/1000 grams of recovery rate are calculated, obtaining recovery rate is 8%；
28 grams of ginkgolic acids are obtained, calculate 28 grams/1000 grams of recovery rate, obtaining recovery rate is 2.8%.
Comparative example 2:(traditional extraction liquid extracts pectin comparative experiments)
(1) picking of ginkgo fruit
Maturity period (fruit yellow, matter is soft, mature) picking in ginkgo is selected, is placed in ventilated environment and stores, it is spare.
(2) gingko episperm pre-processes
Weigh 1000 grams of gingko episperms, by screening removal go rotten, corruption raw material, will be selected after raw material rinse 3
There may be the impurity such as soil, sandstone, iron filings, wind to drench 10min, be crushed raw material using food masher for secondary removal.
(3) pectin leaches
The ratio of 1:10 adds leaching liquid, leaching liquid composition are as follows: sodium phosphate into the raw material of crushing in mass ratio
(Na3PO4) 3%.PH value is adjusted to 2 with hydrochloric acid (HCl), stirs 90min at 80 DEG C.Leaching operation reactor is 3 fixations
Bed reactor, using multi-stage batch counter-current extraction operating procedure；It is molten using plate filter filtering acquisition pectin after leaching
Liquid.
(4) pectin solution decolourizes
Addition active carbon in pectin solution after filtration, and the 60min that decolourizes at 50 DEG C, pectin solution and active carbon
Ratio is 1L:15g.It is filtered after decoloration using plate filter.
(5) pectin solution is concentrated
Filtered pectin solution is cooled to room temperature, and is concentrated using ceramic super-filtering film, and liquor capacity is original after molten contracting
The 30% of liquor capacity, ultrafiltration retaining molecular weight are 300,000, and operating pressure 0.1MPa, operation temperature is room temperature.
(6) pectin ethanol precipitation
95% ethanol solution is added in pectin solution after concentration, controls final concentration of 70% of ethyl alcohol in mixed liquor,
It stirs evenly, adjusts the pH value of mixed liquor to 3.5, stand completely rear filtering to be precipitated in 4 hours, obtain pectin crude extract.
(7) pectin crude extract purifies
Pectin crude extract is purified using ethyl alcohol immersion process, removes small molecule and oil-soluble impurities, concentration of alcohol are followed successively by
Dehydrated alcohol, 90% and 80%, soaking temperature are room temperature, and every section of soaking time is 45min.
(8) pectin is dry
Pectin after purification is dried at 55 DEG C, is then comminuted into pectin powder.
(9) ginkgolic acid leaches
It is that leaching agent is leached that the filter residue obtained after pectin, which is extracted, with ethyl alcohol, and leaching carries out 3 times altogether, and the 1st time using step
Suddenly ethanol solution collected by (6) is carried out as leaching liquid, and ethyl alcohol volumetric concentration is 70%, solid-liquid ratio 1:5, and reflux temperature is
60 DEG C, extraction time 60min；2nd leaching is carried out using ethanol solution collected by step (7) as leaching liquid, ethyl alcohol
Volumetric concentration is 82%, solid-liquid ratio 1:5, and reflux temperature is 60 DEG C, extraction time 60min；3rd leaching is dense using volume
The ethanol solution of degree 90% carries out, solid-liquid ratio 1:5, and reflux temperature is 60 DEG C, extraction time 60min；Collect leaching liquid simultaneously
It is filtered with plate and frame filter press, vacuum distillation obtains ginkgolic acid crude extract.
(10) ginkgolic acid separates
The ginkgolic acid crude extract that step (9) obtains carries out reextraction with petroleum ether, after standing 60min, collects extraction
Liquid carries out chromatography with 101 type large pore resin absorption columns, and volumetric concentration is used to carry out for 50,70%, 90% ethanol solution
Gradient elution, eluting temperature are 30 DEG C, and eluent is dried in vacuo after vacuum distillation concentration, obtain faint yellow ginkgolic acid
Extract.
(9) it calculates recovery rate: obtaining 50 grams of jelly powders.50 grams/1000 grams of recovery rate are calculated, obtaining recovery rate is 5%.?
To 25 grams of ginkgolic acids, 25 grams/1000 grams of recovery rate are calculated, obtaining recovery rate is 2.5%.
Embodiment 2
A kind of gingko episperm pectin and compound of phenolic acid extraction method provided by the invention successively include following step
It is rapid:
(1) picking of ginkgo fruit
It selects to pick in the Chinese olive phase of ginkgo, is placed in ventilated environment and stores, it is spare.
(2) gingko episperm pre-processes
Weigh 1000 grams of gingko episperms, by screening removal go rotten, corruption raw material, will be selected after raw material rinse 3
There may be the impurity such as soil, sandstone, iron filings, wind to drench 10min, be crushed raw material using food masher for secondary removal.
(3) pectin leaches
The ratio of 1:10 adds leaching liquid, leaching liquid composition are as follows: sodium phosphate into the raw material of crushing in mass ratio
(Na3PO4) 8%, disodium hydrogen phosphate (Na2HPO4) 1.5%, sodium citrate (Na3C6H5O7) 100mM, hydroxyacetic acid
(HOCH2COOH) 1%.PH value is adjusted to 2 with hydrochloric acid (HCl), stirs 90min at 80 DEG C.Leaching operation reactor is 4 solid
Fixed bed reactor, using multi-stage batch counter-current extraction operating procedure；Pectin is obtained using plate filter filtering after leaching
Solution.
(4) pectin solution decolourizes
Addition active carbon in pectin solution after filtration, and the 60min that decolourizes at 70 DEG C, pectin solution and active carbon
Ratio is 1L:10g.It is filtered after decoloration using plate filter.
(5) pectin solution is concentrated
Filtered pectin solution is cooled to room temperature, and is concentrated using ceramic super-filtering film, and liquor capacity is original after concentration
The 30% of liquor capacity, ultrafiltration retaining molecular weight are 50,000, and operating pressure 0.2MPa, operation temperature is room temperature.
(6) pectin ethanol precipitation
95% ethanol solution is added in pectin solution after concentration, controls final concentration of 70% of ethyl alcohol in mixed liquor,
It stirs evenly, adjusts the pH value of mixed liquor to 4, stand completely rear filtering to be precipitated in 1 hour, obtain pectin crude extract.
(7) pectin crude extract purifies
Pectin crude extract is purified using ethyl alcohol immersion process, removes small molecule and oil-soluble impurities, concentration of alcohol are followed successively by
Dehydrated alcohol, 90% and 80%, soaking temperature are room temperature, soaking time 60min.
(8) pectin is dry
Pectin after purification is dried at 65 DEG C, is then comminuted into jelly powder.
(9) ginkgolic acid leaches
It is that leaching agent is leached that the filter residue obtained after pectin, which is extracted, with ethyl alcohol, and leaching carries out 3 times altogether, and the 1st time using step
Suddenly ethanol solution collected by (6) is carried out as leaching liquid, and ethyl alcohol volumetric concentration is 70%, solid-liquid ratio 1:5, and reflux temperature is
60 DEG C, extraction time 120min；2nd leaching is carried out using ethanol solution collected by step (7) as leaching liquid, ethyl alcohol
Volumetric concentration is 90%, solid-liquid ratio 1:5, and reflux temperature is 60 DEG C, extraction time 120min；3rd leaching uses volume
The ethanol solution of concentration 95% carries out, solid-liquid ratio 1:5, and reflux temperature is 60 DEG C, extraction time 120min；Collect leaching liquid
And filtered with plate and frame filter press, vacuum distillation obtains ginkgolic acid crude extract.
(10) ginkgolic acid separates
The ginkgolic acid crude extract that step (9) obtains carries out reextraction with petroleum ether, after standing 60min, collects extraction
Liquid carries out chromatography with 101 type large pore resin absorption columns, and volumetric concentration is used to carry out for 50,70%, 90% ethanol solution
Gradient elution, eluting temperature are 30 DEG C, and eluent is dried in vacuo after vacuum distillation concentration, obtain faint yellow ginkgolic acid
Extract.
(11) it calculates recovery rate: obtaining 150 grams of jelly powders.150 grams/1000 grams of recovery rate are calculated, obtaining recovery rate is
15%.34 grams of ginkgolic acids are obtained, calculate 34 grams/1000 grams of recovery rate, obtaining recovery rate is 3.4%.
The comparative example 3:(maturity period picks the gingko episperm of fruit, extracts pectin experiment)
(1) picking of ginkgo fruit
Maturity period (fruit yellow, matter is soft, mature) picking in ginkgo is selected, is placed in ventilated environment and stores, it is spare.
(2) gingko episperm pre-processes
Weigh 1000 grams of gingko episperms, by screening removal go rotten, corruption raw material, will be selected after raw material rinse 3
There may be the impurity such as soil, sandstone, iron filings, wind to drench 10min, be crushed raw material using food masher for secondary removal.
(3) pectin leaches
The ratio of 1:10 adds leaching liquid, leaching liquid composition are as follows: sodium phosphate into the raw material of crushing in mass ratio
(Na3PO4) 8%, disodium hydrogen phosphate (Na2HPO4) 1.5%, sodium citrate (Na3C6H5O7) 100mM, hydroxyacetic acid
(HOCH2COOH) 1%.PH value is adjusted to 2 with hydrochloric acid (HCl), stirs 90min at 80 DEG C.Leaching operation reactor is 4 solid
Fixed bed reactor, using multi-stage batch counter-current extraction operating procedure；Pectin is obtained using plate filter filtering after leaching
Solution.
(4) pectin solution decolourizes
Addition active carbon in pectin solution after filtration, and the 60min that decolourizes at 50 DEG C, pectin solution and active carbon
Ratio is 1L:15g.It is filtered after decoloration using plate filter.
(5) pectin solution is concentrated
Filtered pectin solution is cooled to room temperature, and is concentrated using ceramic super-filtering film, and concentration ratio is original solution body
Long-pending 30%, ultrafiltration retaining molecular weight are 300,000, and operating pressure 0.1MPa, operation temperature is room temperature.
(6) pectin ethanol precipitation
95% ethanol solution is added in pectin solution after concentration, controls final concentration of 70% of ethyl alcohol in mixed liquor,
It stirs evenly, adjusts the pH value of mixed liquor to 3.5, stand completely rear filtering to be precipitated in 4 hours, obtain pectin crude extract.
(7) pectin crude extract purifies
Pectin crude extract is purified using ethyl alcohol immersion process, removes small molecule and oil-soluble impurities, concentration of alcohol are followed successively by
Dehydrated alcohol, 90% and 80%, soaking temperature are room temperature, soaking time 45min.
(8) pectin is dry
Pectin after purification is dried at 55 DEG C, is then comminuted into jelly powder.
(9) ginkgolic acid leaches
It is that leaching agent is leached that the filter residue obtained after pectin, which is extracted, with ethyl alcohol, and leaching carries out 3 times altogether, and the 1st time using step
Suddenly ethanol solution collected by (6) is carried out as leaching liquid, and ethyl alcohol volumetric concentration is 70%, solid-liquid ratio 1:5, and reflux temperature is
60 DEG C, extraction time 120min；2nd leaching is carried out using ethanol solution collected by step (7) as leaching liquid, ethyl alcohol
Volumetric concentration is 90%, solid-liquid ratio 1:5, and reflux temperature is 60 DEG C, extraction time 120min；3rd leaching uses volume
The ethanol solution of concentration 95% carries out, solid-liquid ratio 1:5, and reflux temperature is 60 DEG C, extraction time 120min；Collect leaching liquid
And filtered with plate and frame filter press, vacuum distillation obtains ginkgolic acid crude extract.
(10) ginkgolic acid separates
The ginkgolic acid crude extract that step (9) obtains carries out reextraction with petroleum ether, after standing 60min, collects extraction
Liquid carries out chromatography with 101 type large pore resin absorption columns, and volumetric concentration is used to carry out for 50,70%, 90% ethanol solution
Gradient elution, eluting temperature are 30 DEG C, and eluent is dried in vacuo after vacuum distillation concentration, obtain faint yellow ginkgolic acid
Extract.
(11) it calculates recovery rate: obtaining 76 grams of jelly powders.76 grams/1000 grams of recovery rate are calculated, obtaining recovery rate is
7.6%.31 grams of ginkgolic acids are obtained, calculate 31 grams/1000 grams of recovery rate, obtaining recovery rate is 3.1%.
Comparative example 4:(traditional extraction liquid extracts pectin comparative experiments)
(1) picking of ginkgo fruit
Maturity period (fruit yellow, matter is soft, mature) picking in ginkgo is selected, is placed in ventilated environment and stores, strip
Exosper is spare.
(2) gingko episperm pre-processes
Weigh 1000 grams of gingko episperms, by screening removal go rotten, corruption raw material, will be selected after raw material rinse 3
There may be the impurity such as soil, sandstone, iron filings, wind to drench 10min, be crushed raw material using food masher for secondary removal.
(3) pectin leaches
The ratio of 1:10 adds leaching liquid, leaching liquid composition are as follows: sodium phosphate into the raw material of crushing in mass ratio
(Na3PO4) 8%, pH value is adjusted to 2 with hydrochloric acid (HCl), stirs 90min at 80 DEG C.Leaching operation reactor is 4 fixations
Bed reactor, using multi-stage batch counter-current extraction operating procedure；It is molten using plate filter filtering acquisition pectin after leaching
Liquid.
(4) pectin solution decolourizes
Addition active carbon in pectin solution after filtration, and the 60min that decolourizes at 50 DEG C, pectin solution and active carbon
Ratio is 1L:15g.It is filtered after decoloration using plate filter.
(5) pectin solution is concentrated
Filtered pectin solution is cooled to room temperature, and is concentrated using ceramic super-filtering film, and concentration ratio is original solution body
Long-pending 30%, ultrafiltration retaining molecular weight are 300,000, and operating pressure 0.1MPa, operation temperature is room temperature.
(6) pectin ethanol precipitation
95% ethanol solution is added in pectin solution after concentration, controls final concentration of 70% of ethyl alcohol in mixed liquor,
It stirs evenly, adjusts the pH value of mixed liquor to 3.5, stand completely rear filtering to be precipitated in 4 hours, obtain pectin crude extract.
(7) pectin crude extract purifies
Pectin crude extract is purified using ethyl alcohol immersion process, removes small molecule and oil-soluble impurities, concentration of alcohol are followed successively by
Dehydrated alcohol, 90% and 80%, soaking temperature are room temperature, and immersion elution time is 45min.
(8) pectin is dry
Pectin after purification is dried at 55 DEG C, is then comminuted into jelly powder.
(9) ginkgolic acid leaches
It is that leaching agent is leached that the filter residue obtained after pectin, which is extracted, with ethyl alcohol, and leaching carries out 3 times altogether, and the 1st time using step
Suddenly ethanol solution collected by (6) is carried out as leaching liquid, and ethyl alcohol volumetric concentration is 70%, solid-liquid ratio 1:5, and reflux temperature is
60 DEG C, extraction time 120min；2nd leaching is carried out using ethanol solution collected by step (7) as leaching liquid, ethyl alcohol
Volumetric concentration is 80%, solid-liquid ratio 1:5, and reflux temperature is 60 DEG C, extraction time 120min；3rd leaching uses volume
The ethanol solution of concentration 90% carries out, solid-liquid ratio 1:5, and reflux temperature is 60 DEG C, extraction time 120min；Collect leaching liquid
And filtered with plate and frame filter press, vacuum distillation obtains ginkgolic acid crude extract.
(10) ginkgolic acid separates
The ginkgolic acid crude extract that step (9) obtains carries out reextraction with petroleum ether, after standing 60min, collects extraction
Liquid carries out chromatography with 101 type large pore resin absorption columns, and volumetric concentration is used to carry out for 50,70%, 90% ethanol solution
Gradient elution, eluting temperature are 30 DEG C, and eluent is dried in vacuo after vacuum distillation concentration, obtain faint yellow ginkgolic acid
Extract.
(11) it calculates recovery rate: obtaining 76 grams of jelly powders.76 grams/1000 grams of recovery rate are calculated, obtaining recovery rate is
7.6%.29 grams of ginkgolic acids are obtained, calculate 29 grams/1000 grams of recovery rate, obtaining recovery rate is 2.9%.
Claims (5)
1. a kind of method that gingko episperm extracts pectin and phenolic acid compound simultaneously, which is characterized in that successively include as follows
Step:
(1) picking of ginkgo fruit
Selection picks ginkgo in the Chinese olive phase, and it is spare to strip exosper；
(2) gingko episperm pre-processes
Gingko episperm first pass around screening removal go rotten, corruption raw material, it is selected after starting material with water rinse 2-5 time, wind drench
Then 5-30min is crushed gingko episperm using food masher；
(3) pectin leaches
The ratio of 1:5-1:30 adds leaching liquid, leaching liquid solute composition are as follows: phosphorus into the gingko episperm of crushing in mass ratio
Sour sodium (Na3PO4) 2-8wt%, disodium hydrogen phosphate (Na2HPO4) 0.5-4wt%, sodium citrate (Na3C6H5O7) 10-100mM, hydroxyl
Guanidine-acetic acid (HOCH2COOH) 0.2-1wt%；Leaching liquid salt acid for adjusting pH value to 2-6；The stirring leaching 45- at 70-90 DEG C
120min；Leaching operation reactor is 3-8 fixed bed reactors, using multi-stage batch counter-current extraction operating procedure；Leaching knot
Pectin solution is obtained using plate filter filtering after beam；
(4) pectin solution decolourizes
Active carbon, and the 30-120min that decolourizes under the conditions of 50-70 DEG C of temperature, fruit are added in step (3) filtered pectin solution
The ratio of sol solution and active carbon is 1L:5-20g；Filtering obtains pectin solution；
(5) pectin solution is concentrated
Step (4) filtered pectin solution is cooled to room temperature, and is concentrated using ceramic super-filtering film, liquor capacity is after concentration
The 20-50% of original solution volume before being concentrated, ultrafiltration retaining molecular weight are 10,000-300,000, operating pressure 0.05-
0.3MPa, operation temperature are room temperature；Obtain fructose concentrating liquid；
(6) pectin ethanol precipitation
The ethanol water of volumetric concentration 85-95% is added in step (5) fructose concentrating liquid, controls the whole body of ethyl alcohol in mixed liquor
Product concentration is 50%-80%, is stirred evenly, and adjusts the pH value of mixed liquor to 3-6, stands 0.5-4 hours completely rear mistakes to be precipitated
Filter, solid matter are the pectin crude extract obtained；
(7) pectin crude extract purifies
The pectin crude extract that step (6) obtains is purified using ethyl alcohol immersion process, and it is dense that concentration of alcohol is followed successively by dehydrated alcohol, volume
It spends 88-92% ethanol water and volumetric concentration 78-82% ethanol water, soaking temperature is room temperature, every section of soaking time is
30-90min；
(8) pectin is dry
Pectin after purification is dried at 50-70 DEG C, is then comminuted into pectin powder；
(9) ginkgolic acid leaches
The filter residue that step (3) is obtained by filtration is that leaching agent is leached with ethyl alcohol, and leaching carries out 3 times altogether, and the 1st leaching is using step
Suddenly ethanol solution collected by (6) is carried out as leaching liquid, and ethyl alcohol volumetric concentration is 60-80%, solid-liquid ratio 1:5-15, reflux
Temperature is 50-70 DEG C, extraction time 30-240min；2nd leaching is using ethanol solution collected by step (7) as leaching
Liquid is taken to carry out, ethyl alcohol volumetric concentration is 60-80%, and solid-liquid ratio 1: 5-15, reflux temperature is 50-70 DEG C, extraction time 30-
240min；3rd leaching is carried out using the ethanol solution of volumetric concentration 60-80%, solid-liquid ratio 1:5-15, and reflux temperature is
50-70 DEG C, extraction time 30-240min；It collects leaching liquid and is filtered with plate and frame filter press, vacuum distillation obtains ginkgolic acid
Crude extract；
(10) ginkgolic acid separates
The ginkgolic acid crude extract that step (9) obtains carries out reextraction with petroleum ether, after standing 60-240min, collects extraction
Liquid carries out chromatography with 101 type large pore resin absorption columns, uses volumetric concentration for the second of 45-55%, 65-75%, 85-95%
Alcoholic solution carries out gradient elution, and eluting temperature is 25-55 DEG C, and eluent is dried in vacuo after vacuum distillation concentration, obtains
Faint yellow ginkgolic acid extract.
2. the method that gingko episperm according to claim 1 extracts pectin and compound of phenolic acid simultaneously, it is characterized in that: institute
The Chinese olive phase for stating step (1) ginkgo is the 7-9 month；It is mildew and rot, corruption that step (2) gingko episperm first passes around screening removal
Raw material will be smart to prevent there may be one of soil, sandstone, iron filings impurity or two kinds or more in gingko episperm raw material
Starting material with water after choosing rinses 2-5 times, and wind drenches 5-30min, is then crushed gingko episperm using food masher.
3. the method that gingko episperm according to claim 1 extracts pectin and compound of phenolic acid simultaneously, it is characterized in that: institute
State preferably constituting for step (3) leaching liquid solute are as follows: sodium phosphate (Na3PO4) 3-5wt%, disodium hydrogen phosphate (Na2HPO4)1-
3wt%, sodium citrate (Na3C6H5O7) 40-70mM, hydroxyacetic acid (HOCH2COOH) 0.4-0.7wt%.
4. the method that gingko episperm according to claim 1 extracts pectin and compound of phenolic acid simultaneously, it is characterized in that: institute
Stating step (3) leaching operation reactor is the 3-8 fixed bed reactors successively contacted, and is operated using multi-stage batch counter-current extraction
Technique, the counter-current extraction refer to that material and leaching liquid are flowed at opposite direction, and material is from left side reactor side reaction to the right
Device flowing, leaching liquid is from right side reactor reactor flow to the left；Fruit is obtained using plate filter filtering after leaching
Sol solution.
5. the method that gingko episperm according to claim 1 extracts pectin and compound of phenolic acid simultaneously, it is characterized in that: institute
Step (4) pectin solution is stated using active carbon decoloring, 50-70 DEG C of bleaching temperature, bleaching time 30-120min, pectin solution with
The ratio of active carbon is 1L:5-20g；It is filtered after decoloration using plate filter.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0564572A (en) * | 1991-09-05 | 1993-03-19 | Sanyoo Shokuhin Kk | Soft drink containing ginkgo leaf extract |
| CN1442431A (en) * | 2003-04-02 | 2003-09-17 | 石启田 | Ginkgo pectin extracted by using ginkgo external seed peel as raw material and extraction method |
| CN1763209A (en) * | 2005-09-26 | 2006-04-26 | 江南大学 | Comprehensive utilization process for gingko episperm |
| CN101091730A (en) * | 2006-06-23 | 2007-12-26 | 海南医学院 | Technique for preparing gingkgo extractive with low content of ginkgolic acid |
| CN103749550A (en) * | 2014-01-15 | 2014-04-30 | 东南大学 | Comprehensive utilization method of ginkgo biloba testa |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0564572A (en) * | 1991-09-05 | 1993-03-19 | Sanyoo Shokuhin Kk | Soft drink containing ginkgo leaf extract |
| CN1442431A (en) * | 2003-04-02 | 2003-09-17 | 石启田 | Ginkgo pectin extracted by using ginkgo external seed peel as raw material and extraction method |
| CN1763209A (en) * | 2005-09-26 | 2006-04-26 | 江南大学 | Comprehensive utilization process for gingko episperm |
| CN101091730A (en) * | 2006-06-23 | 2007-12-26 | 海南医学院 | Technique for preparing gingkgo extractive with low content of ginkgolic acid |
| CN103749550A (en) * | 2014-01-15 | 2014-04-30 | 东南大学 | Comprehensive utilization method of ginkgo biloba testa |
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