CN106832045A - 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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Abstract
The invention discloses a kind of method for extracting pectin and phenolic acid compound simultaneously from gingko episperm, it is characterized in that：(1) selection plucks 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 activated carbon decolorizing that leaching is obtained；(5) pectin solution after decolourizing is concentrated using ceramic super-filtering film；(6) pectin solution after concentrating uses ethanol precipitation；(7) pectin crude extract is purified using ethanol 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 carries out chromatography using large pore resin absorption column, is vacuum dried 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 from gingko episperm simultaneously extract pectin and
The method of phenolic acid compound.
Background technology
Ginkgo is Ginkgoaceae ginkgo platymiscium, also known as Gong Sunshu, maidenhair tree, is that the distinctive preciousness of China is medicinal
Plant, its leaf, fruit and exosper etc. all have medicinal Development volue, are referred to as " whole body is all precious living fossil ".
The ginkgo biloba extract preparation developed by ginkgo leaf is one of well received natural drug, is developed by gingko
Various nutraceutical it is also a lot, the utilization rate for having gingko episperm only is relatively low.According to statistics, I
State there are about 30,000 tons or so exospers and is dropped as waste every year, not be exploited, not only waste of resource but also
Pollution environment, and skin contact can also cause the malicious sample dermatitis of paint.Studies have found that gingko episperm is with more
Aspect pharmacological activity, there is value higher, can be used for the exploitation of medicine, health products and plant pesticide,
Have broad application prospects.Therefore, study, develop gingko episperm biological products to comprehensive utilization ginkgo
Resource and preserve the ecological environment it is significant, it has also become the hot subject of current research.Gingko episperm
It is the cortex of food containing gingko almond, i.e. seed duricrust exterior portion is commonly called as gingko afterbirth, and its quality accounts for whole seed
70%.Gingko episperm complicated component, contains various active chemical composition and nutritional ingredient, wherein pectin
It is content composition higher with ginkgolic acid, pectin content can reach ginkgo nut gross weight in gingko episperm
13%, the content of phenolic acid is 3.54%.Pectin is a kind of natural polysaccharide high molecular polymer, is white
To yellowish-brown powder, with colorless and odorless, without the property such as definite melting point and solubility, have insoluble in ethanol etc.
Machine solvent, but hot water is dissolved in, it is slightly soluble in cold water.Pectin is the main of the seventh-largest nutrient diet fiber of human body
Composition, with multiple eating and medical value, has a wide range of applications in food, medicine and other fields.Ginkgo
Contain phenolic acid higher in exosper, ginkgolic acid, hydrogenation gingko can be divided into by the difference of chemical constitution
More than 16 kinds of acid, hydroginkgolinic acid, bilobol, ginkgol etc..It is anti-that research shows that ginkgolic acid has
The effects such as tumour, anti-inflammatory, antiallergy, antibacterial, prevention and elimination of disease and pests, in food, cosmetics, biological pesticide
There is good application value with medicine aspect.
Traditional pectin extraction method has boiling water extraction process, acid hydrolyzation, microbial method, microwave―assisted extraction
Deng, acid extraction method is generally used in industrial production, the method has the low, technique of production equipment requirement simpler
The advantages of pectin quality easy to control, being easy to amplify, obtain is good, purity is high.But also there is high energy consumption, have
The shortcomings of machine solvent load is big, treatment wastewater flow rate is big.Separating Ginkgo phenolic acids compound extracting method is mainly using just
The relatively low organic solvent extraction of hexane, chloroform, ether isopolarity, although the impurity of dissolution is few, but solvent
Permeability is not strong, and consumption is big, and toxicity is also big, relatively costly.The extracting method of current ginkgo product is to carry
Take single substance, such as acidity extraction pectin is that to obtain water-soluble preferably pectin product, phenolic acid etc. water-soluble
The poor compound of property is taken as impurity treatment and falls, and this not only wastes resource and also increases at waste water, waste residue
The difficulty of reason, while solvent utilization rate and production efficiency is not also high.Accordingly, it would be desirable to develop good separating effect,
Extraction efficiency is high, solvent utilization rate is high, cost is relatively low, planted from outside ginkgo with industrialized production future
Pectin and phenolic acid compound new technology and new method are extracted in skin simultaneously.
The content 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 relative
It is low, extract pectin and phenolic acid compound newly side simultaneously from gingko episperm with industrialized production future
Method.
The purpose of the present invention is that development quality is high, extraction efficiency is high, can be planted with outside the ginkgo of industrialized production
Follicarpium glue new method for extracting.
Definition：Gingko episperm：Ginkgo is gymnosperm, and (gingko seed includes to be wrapped in gingko seed
Pulp and shell) outward similar pulp part be exosper.
1st, a kind of gingko episperm pectin extraction and compound of phenolic acid method, it is characterised in that successively including as follows
Step：
(1) harvesting of ginkgo fruit
Selection plucks ginkgo in the Chinese olive phase (the 7-9 months), strips exosper standby；
(2) gingko episperm pretreatment
Gingko episperm first pass around screening removal go rotten, corrupt 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 leaching
In mass ratio 1:5-1:30 ratio adds leaching liquid, leaching liquid solute in the gingko episperm to crushing
Constitute and be：Sodium phosphate (Na3PO4) 2-8wt%, disodium hydrogen phosphate (Na2HPO4) 0.5-4wt%, lemon
Sour sodium (Na3C6H5O7) 10-100mM, hydroxyacetic acid (HOCH2COOH) 0.2-1wt%；Leaching liquid salt
Acid for adjusting pH value is to 2-6；Leaching 45-120min is stirred at 70-90 DEG C；Leaching operation reactor is 3-8
Individual fixed bed reactors, using multi-stage batch counter-current extraction operating procedure (counter-current extraction process refer to material with
Leaching liquid flows into opposite direction, and from left side reactor reactor flow to the right, leaching liquid is from the right side for material
Side reaction device reactor flow to the left)；Leaching obtains pectin solution after terminating using plate filter filtering；
(4) pectin solution decolourizes
Addition activated carbon in pectin solution after step (3) filtering, and decolourized under 50-70 DEG C of temperature conditionss
The ratio of 30-120min, pectin solution and activated carbon is 1L:5-20g；Filtering obtains pectin solution；
(5) pectin solution concentration
Pectin solution after step (4) filtering is cooled to room temperature, is concentrated using ceramic super-filtering film, dense
Liquor capacity is the 20-50% of original solution volume before concentration after contracting, and ultrafiltration retaining molecular weight is
10,000-300,000, operating pressure is 0.05-0.3MPa, and operation temperature is room temperature；Obtain pectin concentration
Liquid；
(6) pectin ethanol precipitation
The ethanol water of volumetric concentration 85-95% is added in step (5) fructose concentrating liquid, mixed liquor is controlled
The final volume concentration of middle ethanol is 50%-80%, is stirred, and adjusts the pH value of mixed liquor to 3-6, is stood
Completely rear filtering to be precipitated in 0.5-4 hours, solid matter is the pectin crude extract of acquisition；
(7) pectin crude extract purifying
The pectin crude extract that step (6) is obtained is purified using ethanol immersion process, and concentration of alcohol is followed successively by nothing
Water-ethanol, volumetric concentration 88-92% ethanol waters and volumetric concentration 78-82% ethanol waters, immersion temperature
It is room temperature to spend, and every section of soak time is 30-90min；
(8) pectin is dried
Pectin after purification is dried at 50-70 DEG C, is then comminuted into pectin powder.
(9) ginkgolic acid leaching
The filter residue that step (3) is filtrated to get is that leaching agent is leached with ethanol, and leaching is carried out 3 times altogether,
1st leaching is carried out using the ethanol solution collected by step (6) as leaching liquid, ethanol volumetric concentration
It is 60-80%, solid-liquid ratio is 1:5-15, reflux temperature is 50-70 DEG C, and extraction time is 30-240min；
2nd leaching is carried out using the ethanol solution collected by step (7) as leaching liquid, ethanol volumetric concentration
It is 60-80%, solid-liquid ratio is 1:5-15, reflux temperature is 50-70 DEG C, and extraction time is 30-240min；
3rd leaching is carried out using the ethanol solution of volumetric concentration 60-80%, and solid-liquid ratio is 1:5-15, backflow temperature
It is 50-70 DEG C to spend, and extraction time is 30-240min；Collect leaching liquid and filtered with plate and frame filter press, subtract
Pressure distillation obtains ginkgolic acid crude extract.
(10) ginkgolic acid is separated
The ginkgolic acid crude extract that step (9) is obtained carries out reextraction with petroleum ether, stands 60-240min
Afterwards, collect extract carries out chromatography with 101 type large pore resin absorption columns, uses concentration to use volume
Concentration carries out gradient elution for the ethanol solution of 45-55%, 65-75%, 85-95%, and eluting temperature is 25-55 DEG C,
Eluent is vacuum dried after being concentrated through vacuum distillation, obtains faint yellow ginkgolic acid extract.
Above-mentioned gingko episperm pectin and ginkgolic acid extracting method, step (1) is：Selection is in ginkgo
The Chinese olive phase (the 7-9 months) pluck, be placed on storage in ventilated environment, standby, exosper is stripped during treatment；
Further, above-mentioned gingko episperm pectin and ginkgolic acid extracting method, step (2) is：
Gingko episperm first pass around screening removal go rotten, corrupt raw material, it is selected after raw material rinse 3 times, wind
10min is drenched, then gingko episperm is crushed using food masher；
Further, above-mentioned gingko episperm pectin and ginkgolic acid extracting method, step (3) is：
In mass ratio 1:5-1:30 ratio is constituted to leaching liquid, leaching liquid is added in the gingko episperm crushed：Phosphorus
Sour sodium (Na3PO4) 2-8%, disodium hydrogen phosphate (Na2HPO4) 0.5-4%, sodium citrate (Na3C6H5O7)
10-100mM, hydroxyacetic acid (HOCH2COOH) 0.2-1%.Leaching operation reactor is that 3-8 fixed bed is anti-
Device is answered, (counter-current extraction process refers to material and leaching liquid into phase using multi-stage batch counter-current extraction operating procedure
Anti- direction flowing, material from left side reactor reactor flow to the right, leaching liquid from right side reactor to
Left side reactor flow)；
Further, above-mentioned gingko episperm pectin and ginkgolic acid extracting method, step (4) is：
Pectin solution uses activated carbon decolorizing, 50-70 DEG C of bleaching temperature, bleaching time 30-120min, pectin solution
It is 1L with the ratio of activated carbon:5-20g；
Further, above-mentioned gingko episperm pectin and ginkgolic acid extracting method, step (5) is：
Pectin solution is concentrated using ceramic super-filtering film, volume is the 20-50% of original solution volume after concentration, milipore filter cuts
It is 10,000-300,000 to stay molecular weight, and operating pressure is 0.05-0.3Mpa；
Further, above-mentioned gingko episperm pectin and ginkgolic acid extracting method, step (6) is：
Fructose concentrating liquid uses ethanol precipitation pectin, and the final volume concentration of ethanol is 50%-80%, and the pH of solution is 3-6,
Time of repose is 0.5-4 hours；
Further, above-mentioned gingko episperm pectin and ginkgolic acid extracting method, step (7) is：
Pectin crude extract is purified using ethanol immersion process, removes small molecule and oil-soluble impurities, and concentration of alcohol is successively
It is absolute ethyl alcohol, volumetric concentration 88-92% ethanol waters and volumetric concentration 78-82% ethanol waters, immersion
Temperature is room temperature, and soak time is 30-90min；
Further, above-mentioned gingko episperm pectin and ginkgolic acid extracting method, step (8) is：
Pectin after purification is dried at 50-70 DEG C, is then comminuted into pectin powder.
Further, above-mentioned gingko episperm pectin and ginkgolic acid extracting method, step (9) is：
The filter residue that step (3) is filtrated to get is that leaching agent is leached with ethanol, and leaching is carried out 3 times altogether, the 1st time
Leaching is carried out using the ethanol solution collected by step (6) as leaching liquid, and ethanol volumetric concentration is 60-80%,
Solid-liquid ratio is 1:5-15, reflux temperature is 50-70 DEG C, and extraction time is 30-240min；2nd leaching is adopted
Carried out as leaching liquid with the ethanol solution collected by step (7), ethanol volumetric concentration is 60-80%, material
Liquor ratio is 1:5-15, reflux temperature is 50-70 DEG C, and extraction time is 30-240min；3rd leaching is used
The ethanol solution of volumetric concentration 60-80% is carried out, and solid-liquid ratio is 1:5-15, reflux temperature is 50-70 DEG C, is carried
The time is taken for 30-240min；Collect leaching liquid and filtered with plate and frame filter press, vacuum distillation obtains ginkgol
Sour crude extract.
Further, above-mentioned gingko episperm pectin and ginkgolic acid extracting method, step (10) is：
The ginkgolic acid crude extract that step (9) is obtained carries out reextraction with petroleum ether, after standing 60-240min,
Collect extract carries out chromatography with 101 type large pore resin absorption columns, uses concentration to use volumetric concentration
For the ethanol solution of 45-55%, 65-75%, 85-95% carries out gradient elution, eluting temperature is 25-55 DEG C,
Eluent is vacuum dried after being concentrated through vacuum distillation, obtains faint yellow ginkgolic acid extract.
Compared with prior art, the technical scheme that the present invention is provided has following technological merit：
(1) it is the Chinese olive phase (the 7-9 months) of fruit, the spy that the period plucks that the present invention chooses gingko episperm
Point is pectin content high, it is easy to store and carry out pre-treatment.
(2) technical scheme that the present invention is provided has prepared a kind of new gingko episperm pectin leaching liquid, can
To improve pectin extraction yield.
(3) the technical scheme pectin leaching that the present invention is provided leaches operating procedure using multi-stage countercurrent, can be with
Pectin extraction yield is improved, while the consumption of leaching liquid can also be reduced, production cost is reduced.
(4) the technical scheme pectin crude extract that the present invention is provided is purified using ethanol immersion process, is removed small
Molecule and oil-soluble impurities, can improve the quality of pectin, and can subtract using multistage dip operation technique
Few ethanol consumption, reducing energy consumption.
(5) technical scheme that the present invention is provided can simultaneously extract pectin and ginkgol in gingko episperm
Acid, improves the utilization rate of gingko resource.
(6) technical scheme that the present invention is provided provides a kind of production work for comprehensively utilizing pectin purification solvent
Skill, can improve solvent utilization rate, reduce solvent usage amount.
Specific embodiment
The present invention is described in detail with reference to specific embodiment.Following examples will be helpful to this area
Technical staff further understand the present invention, but do not constitute any limitation of the invention.Anyone is in this hair
Any type of modification made in bright right, still within the claims in the present invention protection domain.
Embodiment 1
The method that a kind of gingko episperm that the present invention is provided extracts pectin and phenolic acid compound simultaneously, successively
Comprise the following steps：
(1) harvesting of ginkgo fruit
Select the Chinese olive phase (the 7-9 months) in ginkgo to pluck, be placed on storage in ventilated environment；Strip
Exosper is standby.
(2) gingko episperm pretreatment
1000 grams of gingko episperms are weighed, by mildew and rot, the corrupt raw material of screening removal, after selected
Raw material rinses 3 removals and there may be the impurity such as soil, sandstone, iron filings, and wind drenches 10min, using food
Pulverizer crushes raw material.
(3) pectin leaching
In mass ratio 1:10 ratio constitutes and is to leaching liquid, leaching liquid is added in the raw material crushed：Phosphoric acid
Sodium (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), is stirred at 80 DEG C
90min.Leaching operation reactor is 3 fixed bed reactors, using multi-stage batch counter-current extraction operative employee
Skill；Leaching obtains pectin solution after terminating using plate filter filtering.
(4) pectin solution decolourizes
Addition activated carbon in pectin solution after filtration, and the 60min that decolourized at 50 DEG C, pectin solution with
The ratio of activated carbon is 1L:15g.Decolouring is filtered after terminating using plate filter.
(5) pectin solution concentration
Pectin solution after filtering is cooled to room temperature, is concentrated using ceramic super-filtering film, solution body after concentration
Product is the 30% of original solution volume, and ultrafiltration retaining molecular weight is 300,000, and operating pressure is 0.1MPa,
Operation temperature is room temperature.
(6) pectin ethanol precipitation
95% ethanol solution is added in pectin solution after concentration, ethanol is final concentration of in control mixed liquor
70%, stir, adjust the pH value of mixed liquor to 3.5 with hydrochloric acid (HCl), stand 4 hours it is to be precipitated
Filtering after completely, obtains pectin crude extract.
(7) pectin crude extract purifying
Pectin crude extract is purified using ethanol immersion process, removes small molecule and oil-soluble impurities, concentration of alcohol
Absolute ethyl alcohol, 90% and 80% are followed successively by, soaking temperature is room temperature, and every section of soak time is 45min.
(8) pectin is dried
Pectin after purification is dried at 55 DEG C, is then comminuted into pectin powder.
(9) ginkgolic acid leaching
It is that leaching agent is leached with ethanol to extract the filter residue obtained after pectin, and leaching carries out 3 times, the 1st altogether
Ethanol solution collected by secondary use step (6) is carried out as leaching liquid, and ethanol volumetric concentration is 70%, material
Liquor ratio is 1:5, reflux temperature is 60 DEG C, and extraction time is 60min；2nd leaching is using step (7)
Collected ethanol solution is carried out as leaching liquid, and ethanol volumetric concentration is 85%, and solid-liquid ratio is 1:5, return
Stream temperature is 60 DEG C, and extraction time is 60min；3rd leaching uses the ethanol solution of volumetric concentration 95%
Carry out, solid-liquid ratio is 1:5, reflux temperature is 60 DEG C, and extraction time is 120min；Leaching liquid is collected to be used in combination
Plate and frame filter press is filtered, and vacuum distillation obtains ginkgolic acid crude extract.
(10) ginkgolic acid is separated
The ginkgolic acid crude extract that step (9) is obtained carries out reextraction with petroleum ether, after standing 60min,
Collect extract carries out chromatography with 101 type large pore resin absorption columns, use volumetric concentration for 50,70%,
90% ethanol solution carries out gradient elution, and eluting temperature is 30 DEG C, and eluent concentrates laggard through vacuum distillation
Row vacuum drying, obtains faint yellow ginkgolic acid extract.
(11) recovery rate is calculated：130 grams of jelly powders are obtained, 130 grams/1000 grams of recovery rate is calculated, obtained
It is 13% to recovery rate；32 grams of ginkgolic acids are obtained, 32 grams/1000 grams of recovery rate is calculated, is extracted
Rate is 3.2%.
Comparative example 1：(maturity period plucks the gingko episperm of fruit, extracts pectin experiment)
(1) harvesting of ginkgo fruit
Select the maturity period (fruit yellow, matter is soft, ripe) in ginkgo to pluck, be placed on ventilation
Stored in environment, strip exosper standby.
(2) gingko episperm pretreatment
1000 grams of gingko episperms are weighed, by mildew and rot, the corrupt raw material of screening removal, after selected
Raw material rinses 3 removals and there may be the impurity such as soil, sandstone, iron filings, and wind drenches 10min, using food
Pulverizer crushes raw material.
(3) pectin leaching
In mass ratio 1:10 ratio constitutes and is to leaching liquid, leaching liquid is added in the raw material crushed：Phosphoric acid
Sodium (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), is stirred at 80 DEG C
90min.Leaching operation reactor is 3 fixed bed reactors, using multi-stage batch counter-current extraction operative employee
Skill；Leaching obtains pectin solution after terminating using plate filter filtering.
(4) pectin solution decolourizes
Addition activated carbon in pectin solution after filtration, and the 60min that decolourized at 50 DEG C, pectin solution with
The ratio of activated carbon is 1L:15g.Decolouring is filtered after terminating using plate filter.
(5) pectin solution concentration
Pectin solution after filtering is cooled to room temperature, is concentrated using ceramic super-filtering film, solution body after molten contracting
Product is the 30% of original solution volume, and ultrafiltration retaining molecular weight is 300,000, and operating pressure is 0.1MPa,
Operation temperature is room temperature.
(6) pectin ethanol precipitation
95% ethanol solution is added in pectin solution after concentration, ethanol is final concentration of in control mixed liquor
70%, stir, the pH value of mixed liquor is adjusted to 3.5, completely rear filtering to be precipitated in 4 hours is stood,
Obtain pectin crude extract.
(7) pectin crude extract purifying
Pectin crude extract is purified using ethanol immersion process, removes small molecule and oil-soluble impurities, concentration of alcohol
Absolute ethyl alcohol, 90% and 80% are followed successively by, soaking temperature is room temperature, and soak time is 45min.
(8) pectin is dried
Pectin after purification is dried at 55 DEG C, is then comminuted into pectin powder.
(9) ginkgolic acid leaching
It is that leaching agent is leached with ethanol to extract the filter residue obtained after pectin, and leaching carries out 3 times, the 1st altogether
Ethanol solution collected by secondary use step (6) is carried out as leaching liquid, and ethanol volumetric concentration is 70%, material
Liquor ratio is 1:5, reflux temperature is 60 DEG C, and extraction time is 60min；2nd leaching is using step (7)
Collected ethanol solution is carried out as leaching liquid, and ethanol volumetric concentration is 85%, and solid-liquid ratio is 1:5, return
Stream temperature is 60 DEG C, and extraction time is 60min；3rd leaching uses the ethanol solution of volumetric concentration 95%
Carry out, solid-liquid ratio is 1:5, reflux temperature is 60 DEG C, and extraction time is 120min；Leaching liquid is collected to be used in combination
Plate and frame filter press is filtered, and vacuum distillation obtains ginkgolic acid crude extract.
(10) ginkgolic acid is separated
The ginkgolic acid crude extract that step (9) is obtained carries out reextraction with petroleum ether, after standing 60min,
Collect extract carries out chromatography with 101 type large pore resin absorption columns, use volumetric concentration for 50,70%,
90% ethanol solution carries out gradient elution, and eluting temperature is 30 DEG C, and eluent concentrates laggard through vacuum distillation
Row vacuum drying, obtains faint yellow ginkgolic acid extract.
(11) recovery rate is calculated：Obtain 80 grams of jelly powders.80 grams/1000 grams of recovery rate is calculated, is obtained
Recovery rate is 8%；28 grams of ginkgolic acids are obtained, 28 grams/1000 grams of recovery rate is calculated, obtaining recovery rate is
2.8%.
Comparative example 2：(traditional extraction liquid extracts pectin contrast experiment)
(1) harvesting of ginkgo fruit
Select the maturity period (fruit yellow, matter is soft, ripe) in ginkgo to pluck, be placed on ventilation
Stored in environment, it is standby.
(2) gingko episperm pretreatment
1000 grams of gingko episperms are weighed, by mildew and rot, the corrupt raw material of screening removal, after selected
Raw material rinses 3 removals and there may be the impurity such as soil, sandstone, iron filings, and wind drenches 10min, using food
Pulverizer crushes raw material.
(3) pectin leaching
In mass ratio 1:10 ratio constitutes and is to leaching liquid, leaching liquid is added in the raw material crushed：Phosphoric acid
Sodium (Na3PO4) 3%.PH value is adjusted to 2 with hydrochloric acid (HCl), and 90min is stirred at 80 DEG C.Leaching
Operation reactor is 3 fixed bed reactors, using multi-stage batch counter-current extraction operating procedure；Leaching terminates
Pectin solution is obtained using plate filter filtering afterwards.
(4) pectin solution decolourizes
Addition activated carbon in pectin solution after filtration, and the 60min that decolourized at 50 DEG C, pectin solution with
The ratio of activated carbon is 1L:15g.Decolouring is filtered after terminating using plate filter.
(5) pectin solution concentration
Pectin solution after filtering is cooled to room temperature, is concentrated using ceramic super-filtering film, solution body after molten contracting
Product is the 30% of original solution volume, and ultrafiltration retaining molecular weight is 300,000, and operating pressure is 0.1MPa,
Operation temperature is room temperature.
(6) pectin ethanol precipitation
95% ethanol solution is added in pectin solution after concentration, ethanol is final concentration of in control mixed liquor
70%, stir, the pH value of mixed liquor is adjusted to 3.5, completely rear filtering to be precipitated in 4 hours is stood,
Obtain pectin crude extract.
(7) pectin crude extract purifying
Pectin crude extract is purified using ethanol immersion process, removes small molecule and oil-soluble impurities, concentration of alcohol
Absolute ethyl alcohol, 90% and 80% are followed successively by, soaking temperature is room temperature, and every section of soak time is 45min.
(8) pectin is dried
Pectin after purification is dried at 55 DEG C, is then comminuted into pectin powder.
(9) ginkgolic acid leaching
It is that leaching agent is leached with ethanol to extract the filter residue obtained after pectin, and leaching carries out 3 times, the 1st altogether
Ethanol solution collected by secondary use step (6) is carried out as leaching liquid, and ethanol volumetric concentration is 70%, material
Liquor ratio is 1:5, reflux temperature is 60 DEG C, and extraction time is 60min；2nd leaching is using step (7)
Collected ethanol solution is carried out as leaching liquid, and ethanol volumetric concentration is 82%, and solid-liquid ratio is 1:5, return
Stream temperature is 60 DEG C, and extraction time is 60min；3rd leaching uses the ethanol solution of volumetric concentration 90%
Carry out, solid-liquid ratio is 1:5, reflux temperature is 60 DEG C, and extraction time is 60min；Leaching liquid is collected to be used in combination
Plate and frame filter press is filtered, and vacuum distillation obtains ginkgolic acid crude extract.
(10) ginkgolic acid is separated
The ginkgolic acid crude extract that step (9) is obtained carries out reextraction with petroleum ether, after standing 60min,
Collect extract carries out chromatography with 101 type large pore resin absorption columns, use volumetric concentration for 50,70%,
90% ethanol solution carries out gradient elution, and eluting temperature is 30 DEG C, and eluent concentrates laggard through vacuum distillation
Row vacuum drying, obtains faint yellow ginkgolic acid extract.
(9) recovery rate is calculated：Obtain 50 grams of jelly powders.50 grams/1000 grams of recovery rate is calculated, is carried
It is 5% to take rate.25 grams of ginkgolic acids are obtained, 25 grams/1000 grams of recovery rate is calculated, it is 2.5% to obtain recovery rate.
Embodiment 2
A kind of gingko episperm pectin and compound of phenolic acid extracting method that the present invention is provided, successively including as follows
Step：
(1) harvesting of ginkgo fruit
Select the Chinese olive phase in ginkgo to pluck, be placed on storage in ventilated environment, it is standby.
(2) gingko episperm pretreatment
1000 grams of gingko episperms are weighed, by mildew and rot, the corrupt raw material of screening removal, after selected
Raw material rinses 3 removals and there may be the impurity such as soil, sandstone, iron filings, and wind drenches 10min, using food
Pulverizer crushes raw material.
(3) pectin leaching
In mass ratio 1:10 ratio constitutes and is to leaching liquid, leaching liquid is added in the raw material crushed：Phosphoric acid
Sodium (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), and 90min is stirred at 80 DEG C.
Leaching operation reactor is 4 fixed bed reactors, using multi-stage batch counter-current extraction operating procedure；Leaching
Pectin solution is obtained using plate filter filtering after end.
(4) pectin solution decolourizes
Addition activated carbon in pectin solution after filtration, and the 60min that decolourized at 70 DEG C, pectin solution with
The ratio of activated carbon is 1L:10g.Decolouring is filtered after terminating using plate filter.
(5) pectin solution concentration
Pectin solution after filtering is cooled to room temperature, is concentrated using ceramic super-filtering film, solution body after concentration
Product is the 30% of original solution volume, and ultrafiltration retaining molecular weight is 50,000, and operating pressure is 0.2MPa, behaviour
Make temperature for room temperature.
(6) pectin ethanol precipitation
95% ethanol solution is added in pectin solution after concentration, ethanol is final concentration of in control mixed liquor
70%, stir, the pH value of mixed liquor is adjusted to 4, completely rear filtering to be precipitated in 1 hour is stood, obtain
Obtain pectin crude extract.
(7) pectin crude extract purifying
Pectin crude extract is purified using ethanol immersion process, removes small molecule and oil-soluble impurities, concentration of alcohol
Absolute ethyl alcohol, 90% and 80% are followed successively by, soaking temperature is room temperature, and soak time is 60min.
(8) pectin is dried
Pectin after purification is dried at 65 DEG C, is then comminuted into jelly powder.
(9) ginkgolic acid leaching
It is that leaching agent is leached with ethanol to extract the filter residue obtained after pectin, and leaching carries out 3 times, the 1st altogether
Ethanol solution collected by secondary use step (6) is carried out as leaching liquid, and ethanol volumetric concentration is 70%, material
Liquor ratio is 1:5, reflux temperature is 60 DEG C, and extraction time is 120min；2nd leaching is using step (7)
Collected ethanol solution is carried out as leaching liquid, and ethanol volumetric concentration is 90%, and solid-liquid ratio is 1:5, return
Stream temperature is 60 DEG C, and extraction time is 120min；3rd leaching uses the ethanol solution of volumetric concentration 95%
Carry out, solid-liquid ratio is 1:5, reflux temperature is 60 DEG C, and extraction time is 120min；Leaching liquid is collected to be used in combination
Plate and frame filter press is filtered, and vacuum distillation obtains ginkgolic acid crude extract.
(10) ginkgolic acid is separated
The ginkgolic acid crude extract that step (9) is obtained carries out reextraction with petroleum ether, stands 60min
Afterwards, collect extract carries out chromatography with 101 type large pore resin absorption columns, use volumetric concentration for 50,
70%th, 90% ethanol solution carries out gradient elution, and eluting temperature is 30 DEG C, and eluent is concentrated through vacuum distillation
After be vacuum dried, obtain faint yellow ginkgolic acid extract.
(11) recovery rate is calculated：Obtain 150 grams of jelly powders.150 grams/1000 grams of recovery rate is calculated, is obtained
It is 15% to recovery rate.34 grams of ginkgolic acids are obtained, 34 grams/1000 grams of recovery rate is calculated, is extracted
Rate is 3.4%.
Comparative example 1：(maturity period plucks the gingko episperm of fruit, extracts pectin experiment)
(1) harvesting of ginkgo fruit
Select the maturity period (fruit yellow, matter is soft, ripe) in ginkgo to pluck, be placed on ventilation
Stored in environment, it is standby.
(2) gingko episperm pretreatment
1000 grams of gingko episperms are weighed, by mildew and rot, the corrupt raw material of screening removal, after selected
Raw material rinses 3 removals and there may be the impurity such as soil, sandstone, iron filings, and wind drenches 10min, using food
Pulverizer crushes raw material.
(3) pectin leaching
In mass ratio 1:10 ratio constitutes and is to leaching liquid, leaching liquid is added in the raw material crushed：Phosphoric acid
Sodium (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), and 90min is stirred at 80 DEG C.
Leaching operation reactor is 4 fixed bed reactors, using multi-stage batch counter-current extraction operating procedure；Leaching
Pectin solution is obtained using plate filter filtering after end.
(4) pectin solution decolourizes
Addition activated carbon in pectin solution after filtration, and the 60min that decolourized at 50 DEG C, pectin solution with
The ratio of activated carbon is 1L:15g.Decolouring is filtered after terminating using plate filter.
(5) pectin solution concentration
Pectin solution after filtering is cooled to room temperature, is concentrated using ceramic super-filtering film, and concentration ratio is original
The 30% of liquor capacity, ultrafiltration retaining molecular weight is 300,000, and operating pressure is 0.1MPa, operation temperature
It is room temperature to spend.
(6) pectin ethanol precipitation
95% ethanol solution is added in pectin solution after concentration, ethanol is final concentration of in control mixed liquor
70%, stir, the pH value of mixed liquor is adjusted to 3.5, completely rear filtering to be precipitated in 4 hours is stood,
Obtain pectin crude extract.
(7) pectin crude extract purifying
Pectin crude extract is purified using ethanol immersion process, removes small molecule and oil-soluble impurities, concentration of alcohol
Absolute ethyl alcohol, 90% and 80% are followed successively by, soaking temperature is room temperature, and soak time is 45min.
(8) pectin is dried
Pectin after purification is dried at 55 DEG C, is then comminuted into jelly powder.
(9) ginkgolic acid leaching
It is that leaching agent is leached with ethanol to extract the filter residue obtained after pectin, and leaching carries out 3 times, the 1st altogether
Ethanol solution collected by secondary use step (6) is carried out as leaching liquid, and ethanol volumetric concentration is 70%, material
Liquor ratio is 1:5, reflux temperature is 60 DEG C, and extraction time is 120min；2nd leaching is using step (7)
Collected ethanol solution is carried out as leaching liquid, and ethanol volumetric concentration is 90%, and solid-liquid ratio is 1:5, return
Stream temperature is 60 DEG C, and extraction time is 120min；3rd leaching uses the ethanol solution of volumetric concentration 95%
Carry out, solid-liquid ratio is 1:5, reflux temperature is 60 DEG C, and extraction time is 120min；Leaching liquid is collected to be used in combination
Plate and frame filter press is filtered, and vacuum distillation obtains ginkgolic acid crude extract.
(10) ginkgolic acid is separated
The ginkgolic acid crude extract that step (9) is obtained carries out reextraction with petroleum ether, stands 60min
Afterwards, collect extract carries out chromatography with 101 type large pore resin absorption columns, use volumetric concentration for 50,
70%th, 90% ethanol solution carries out gradient elution, and eluting temperature is 30 DEG C, and eluent is concentrated through vacuum distillation
After be vacuum dried, obtain faint yellow ginkgolic acid extract.
(11) recovery rate is calculated：Obtain 76 grams of jelly powders.76 grams/1000 grams of recovery rate is calculated, is obtained
Recovery rate is 7.6%.31 grams of ginkgolic acids are obtained, 31 grams/1000 grams of recovery rate is calculated, recovery rate is obtained
It is 3.1%.
Comparative example 2：(traditional extraction liquid extracts pectin contrast experiment)
(1) harvesting of ginkgo fruit
Select the maturity period (fruit yellow, matter is soft, ripe) in ginkgo to pluck, be placed on ventilation
Stored in environment, strip exosper standby.
(2) gingko episperm pretreatment
1000 grams of gingko episperms are weighed, by mildew and rot, the corrupt raw material of screening removal, after selected
Raw material rinses 3 removals and there may be the impurity such as soil, sandstone, iron filings, and wind drenches 10min, using food
Pulverizer crushes raw material.
(3) pectin leaching
In mass ratio 1:10 ratio constitutes and is to leaching liquid, leaching liquid is added in the raw material crushed：Phosphoric acid
Sodium (Na3PO4) 8%, pH value is adjusted to 2 with hydrochloric acid (HCl), and 90min is stirred at 80 DEG C.Leaching
Operation reactor is 4 fixed bed reactors, using multi-stage batch counter-current extraction operating procedure；Leaching terminates
Pectin solution is obtained using plate filter filtering afterwards.
(4) pectin solution decolourizes
Addition activated carbon in pectin solution after filtration, and the 60min that decolourized at 50 DEG C, pectin solution with
The ratio of activated carbon is 1L:15g.Decolouring is filtered after terminating using plate filter.
(5) pectin solution concentration
Pectin solution after filtering is cooled to room temperature, is concentrated using ceramic super-filtering film, and concentration ratio is original
The 30% of liquor capacity, ultrafiltration retaining molecular weight is 300,000, and operating pressure is 0.1MPa, operation temperature
It is room temperature to spend.
(6) pectin ethanol precipitation
95% ethanol solution is added in pectin solution after concentration, ethanol is final concentration of in control mixed liquor
70%, stir, the pH value of mixed liquor is adjusted to 3.5, completely rear filtering to be precipitated in 4 hours is stood,
Obtain pectin crude extract.
(7) pectin crude extract purifying
Pectin crude extract is purified using ethanol immersion process, removes small molecule and oil-soluble impurities, concentration of alcohol
Absolute ethyl alcohol, 90% and 80% are followed successively by, soaking temperature is room temperature, immersion elution time is 45min.
(8) pectin is dried
Pectin after purification is dried at 55 DEG C, is then comminuted into jelly powder.
(9) ginkgolic acid leaching
It is that leaching agent is leached with ethanol to extract the filter residue obtained after pectin, and leaching carries out 3 times, the 1st altogether
Ethanol solution collected by secondary use step (6) is carried out as leaching liquid, and ethanol volumetric concentration is 70%, material
Liquor ratio is 1:5, reflux temperature is 60 DEG C, and extraction time is 120min；2nd leaching is using step (7)
Collected ethanol solution is carried out as leaching liquid, and ethanol volumetric concentration is 80%, and solid-liquid ratio is 1:5, return
Stream temperature is 60 DEG C, and extraction time is 120min；3rd leaching uses the ethanol solution of volumetric concentration 90%
Carry out, solid-liquid ratio is 1:5, reflux temperature is 60 DEG C, and extraction time is 120min；Leaching liquid is collected to be used in combination
Plate and frame filter press is filtered, and vacuum distillation obtains ginkgolic acid crude extract.
(10) ginkgolic acid is separated
The ginkgolic acid crude extract that step (9) is obtained carries out reextraction with petroleum ether, after standing 60min,
Collect extract carries out chromatography with 101 type large pore resin absorption columns, use volumetric concentration for 50,70%,
90% ethanol solution carries out gradient elution, and eluting temperature is 30 DEG C, and eluent concentrates laggard through vacuum distillation
Row vacuum drying, obtains faint yellow ginkgolic acid extract.
(11) recovery rate is calculated：Obtain 76 grams of jelly powders.76 grams/1000 grams of recovery rate is calculated, is obtained
Recovery rate is 7.6%.29 grams of ginkgolic acids are obtained, 29 grams/1000 grams of recovery rate is calculated, recovery rate is obtained
It is 2.9%.
Claims (10)
1. a kind of method that gingko episperm extracts pectin and phenolic acid compound simultaneously, it is characterised in that
In turn include the following steps：
(1) harvesting of ginkgo fruit
Selection plucks ginkgo in the Chinese olive phase, strips exosper standby；
(2) gingko episperm pretreatment
Gingko episperm first pass around screening removal go rotten, corrupt raw material, it is selected after starting material with water punching
Wash 2-5 times, wind drenches 5-30min, is then crushed gingko episperm using food masher；
(3) pectin leaching
In mass ratio 1:5-1:30 ratio adds leaching liquid, leaching liquid in the gingko episperm to crushing
Solute is constituted：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；Leaching 45-120min is stirred at 70-90 DEG C；Leaching operation is anti-
Device is answered for 3-8 fixed bed reactors, using multi-stage batch counter-current extraction operating procedure；After leaching terminates
Pectin solution is obtained using plate filter filtering；
(4) pectin solution decolourizes
Addition activated carbon in pectin solution after step (3) filtering, and taken off under 50-70 DEG C of temperature conditionss
The ratio of color 30-120min, pectin solution and activated carbon is 1L:5-20g；Filtering obtains pectin solution；
(5) pectin solution concentration
Pectin solution after step (4) filtering is cooled to room temperature, is concentrated using ceramic super-filtering film,
Liquor capacity is the 20-50% of original solution volume before concentration after concentration, and ultrafiltration retaining molecular weight is
10,000-300,000, operating pressure is 0.05-0.3MPa, and operation temperature is room temperature；Obtain pectin dense
Contracting liquid；
(6) pectin ethanol precipitation
The ethanol water of volumetric concentration 85-95%, control mixing are added in step (5) fructose concentrating liquid
The final volume concentration of ethanol is 50%-80% in liquid, is stirred, and adjusts the pH value of mixed liquor to 3-6,
Completely rear filtering to be precipitated in 0.5-4 hours is stood, solid matter is the pectin crude extract of acquisition；
(7) pectin crude extract purifying
The pectin crude extract that step (6) is obtained is purified using ethanol immersion process, and concentration of alcohol is followed successively by
Absolute ethyl alcohol, volumetric concentration 88-92% ethanol waters and volumetric concentration 78-82% ethanol waters, leaching
Bubble temperature is room temperature, and every section of soak time is 30-90min；
(8) pectin is dried
Pectin after purification is dried at 50-70 DEG C, is then comminuted into pectin powder；
(9) ginkgolic acid leaching
The filter residue that step (3) is filtrated to get is that leaching agent is leached with ethanol, and leaching is carried out 3 times altogether,
1st leaching is carried out using the ethanol solution collected by step (6) as leaching liquid, and ethanol volume is dense
It is 60-80% to spend, and solid-liquid ratio is 1:5-15, reflux temperature is 50-70 DEG C, and extraction time is 30-240min；
2nd leaching is carried out using the ethanol solution collected by step (7) as leaching liquid, and ethanol volume is dense
It is 60-80% to spend, and solid-liquid ratio is 1: 5-15, and reflux temperature is 50-70 DEG C, and extraction time is 30-240min；
3rd leaching is carried out using the ethanol solution of volumetric concentration 60-80%, and solid-liquid ratio is 1:5-15, backflow
Temperature is 50-70 DEG C, and extraction time is 30-240min；Collect leaching liquid and filtered with plate and frame filter press,
Vacuum distillation obtains ginkgolic acid crude extract；
(10) ginkgolic acid is separated
The ginkgolic acid crude extract that step (9) is obtained carries out reextraction with petroleum ether, stands 60-240min
Afterwards, collect extract carries out chromatography with 101 type large pore resin absorption columns, uses concentration to use body
Product concentration carries out gradient elution for the ethanol solution of 45-55%, 65-75%, 85-95%, and eluting temperature is
25-55 DEG C, eluent is vacuum dried after being concentrated through vacuum distillation, is obtained faint yellow ginkgolic acid and is carried
Take thing.
2. gingko episperm pectin according to claim 1 and compound of phenolic acid extracting method, its
It is characterized in：The Chinese olive phase of step (1) ginkgo is the 7-9 months；Step (2) gingko episperm
Mildew and rot, the corrupt raw material of screening removal is first passed around, to prevent there may be mud in gingko episperm raw material
One or two or more kinds in the impurity such as soil, sandstone, iron filings, will be selected after starting material with water rinse 2-5
Secondary, wind drenches 5-30min, is then crushed gingko episperm using food masher.
3. gingko episperm pectin according to claim 1 and compound of phenolic acid extracting method, its
It is characterized in：Step (3) the leaching liquid solute preferably constitute for：Sodium phosphate (Na3PO4) 3-5wt%,
Disodium hydrogen phosphate (Na2HPO4) 1-3wt%, sodium citrate (Na3C6H5O7) 40-70mM, hydroxyacetic acid
(HOCH2COOH) 0.4-0.7wt%.
4. gingko episperm pectin according to claim 1 and compound of phenolic acid extracting method, its
It is characterized in：Step (3) the leaching operation reactor is the 3-8 fixed bed reactors contacted successively,
Using multi-stage batch counter-current extraction operating procedure, (counter-current extraction process refers to material with leaching liquid into opposite
Direction is flowed, material from left side reactor reactor flow to the right, leaching liquid from right side reactor to the left
Side reaction device flows)；Leaching obtains pectin solution after terminating using plate filter filtering.
5. gingko episperm pectin according to claim 1 and compound of phenolic acid extracting method, its
It is characterized in：Step (4) pectin solution uses activated carbon decolorizing, 50-70 DEG C of bleaching temperature to decolourize
The ratio of time 30-120min, pectin solution and activated carbon is 1L:5-20g；Decolouring uses plate after terminating
Frame filter is filtered.
6. gingko episperm pectin according to claim 1 and compound of phenolic acid extracting method, its
It is characterized in：The step (5) concentrates pectin solution using ceramic super-filtering film, and volume is former molten after concentration
The 20-50% of liquid product, ultrafiltration retaining molecular weight is 10,000-300,000, and operating pressure is 0.
05-0.3Mpa。
7. gingko episperm pectin according to claim 1 and compound of phenolic acid extracting method, its
It is characterized in：Step (6) fructose concentrating liquid uses ethanol precipitation pectin, the final volume concentration of ethanol
It is 50%-80%, the pH of solution is 3-6, and time of repose is 0.5-4 hours, and solid matter is acquisition
Pectin crude extract.
8. gingko episperm pectin according to claim 1 and compound of phenolic acid extracting method, its
It is characterized in：Step (7) the pectin crude extract using ethanol immersion process purify, removal small molecule and
Oil-soluble impurities, concentration of alcohol is followed successively by absolute ethyl alcohol, volumetric concentration 88-92% ethanol waters and volume
Concentration 78-82% ethanol waters, soaking temperature is room temperature, and every section of soak time is 30-90min.
9. gingko episperm pectin according to claim 1 and compound of phenolic acid extracting method, its
It is characterized in：It is that leaching agent is leached with ethanol that the step (9) extracts the filter residue obtained after pectin,
Leaching is carried out 3 times altogether, and the 1st leaching is using the ethanol solution collected by step (6) as leaching liquid
Carry out, ethanol volumetric concentration is 60-80%, and solid-liquid ratio is 1:5-15, reflux temperature is 50-70 DEG C, is carried
The time is taken for 30-240min；2nd leaching is using the ethanol solution collected by step (7) as leaching
Liquid is carried out, and ethanol volumetric concentration is 60-80%, and solid-liquid ratio is 1:5-15, reflux temperature is 50-70 DEG C,
Extraction time is 30-240min；3rd leaching is carried out using the ethanol solution of volumetric concentration 60-80%,
Solid-liquid ratio is 1:5-15, reflux temperature is 50-70 DEG C, and extraction time is 30-240min；Collect leaching
Liquid is simultaneously filtered with plate and frame filter press, and vacuum distillation obtains ginkgolic acid crude extract.
10. gingko episperm pectin according to claim 1 and compound of phenolic acid extracting method, its
It is characterized in：Step (10) the ginkgolic acid crude extract carries out reextraction with petroleum ether, stands
After 60-240min, collect extract carries out chromatography with 101 type large pore resin absorption columns, using dense
Degree is to use the volumetric concentration to carry out gradient elution for the ethanol solution of 45-55%, 65-75%, 85-95%, is washed
De- temperature is 25-55 DEG C, and eluent is vacuum dried after being concentrated through vacuum distillation, obtains faint yellow silver
Apricot phenolic acid extract.
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| CN109258703A (en) * | 2018-11-07 | 2019-01-25 | 临沂大学 | A kind of ginkgolic acid-rhamnolipid compound disinfectant and its preparation method and application |
| CN109287665A (en) * | 2018-09-25 | 2019-02-01 | 临沂大学 | A kind of ginkgolic acid-avermectin composite insecticide and preparation method thereof |
| CN113827625A (en) * | 2021-08-15 | 2021-12-24 | 江苏蓝星生物工程有限公司 | Process for preparing high-purity ginkgolic acid extract by using ginkgo episperms |
| CN114794153A (en) * | 2022-05-20 | 2022-07-29 | 贵州北极兴药业有限公司 | Method for recovering ginkgolic acid from waste residues in production of ginkgo biloba extract |
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| 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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| CN113827625A (en) * | 2021-08-15 | 2021-12-24 | 江苏蓝星生物工程有限公司 | Process for preparing high-purity ginkgolic acid extract by using ginkgo episperms |
| CN114794153A (en) * | 2022-05-20 | 2022-07-29 | 贵州北极兴药业有限公司 | Method for recovering ginkgolic acid from waste residues in production of ginkgo biloba extract |
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