CN109810789A - A kind of extracting method of ginkgo essential oil - Google Patents
A kind of extracting method of ginkgo essential oil Download PDFInfo
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- CN109810789A CN109810789A CN201810826937.2A CN201810826937A CN109810789A CN 109810789 A CN109810789 A CN 109810789A CN 201810826937 A CN201810826937 A CN 201810826937A CN 109810789 A CN109810789 A CN 109810789A
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Abstract
The present invention is on the basis of ultrasonic vibration-Multi-stage spiral isolation technics removing plumule, using supercritical CO2Extraction obtains ginkgo essential oil with molecular distillation integrated technology, reaches separation impurity, toxic component is down to extremely low level, ensure that safe edible by the purpose of enrichment function substance.Unsaturated fatty acid accounts for total fatty acids > 92%, general flavone > 0.10%, contains Bilobalide and Ginkgolide A. B. C in the extracted ginkgo essential oil of extracting method of the present invention, total terpene lactone > 0.02%, contain xanthophyll, β-and alpha-carotene, 1 ㎎ of carotenoid total amount >/100g.Above-mentioned functional materials, which have, to delay senescence, reduces the multiple biological functions such as content, anti-oxidant, anticancer of total cholesterol in blood, has fabulous intervention effect to cardiovascular and cerebrovascular disease and improvement neurodegenerative disease.
Description
Technical field
The present invention relates to plants essential oil extractive technique field more particularly to a kind of extracting methods of ginkgo essential oil.
Background technique
Ginkgo nut is commonly called as gingko (Ginkgo Semen), is the dry mature seed of ginkgo (Ginkgo biloba L.),
It is famous one of nut.
Deng Ganchun, Zeng Changmin, Tian Binqiang etc. " extraction of Ginkgo oil and fatty acid compositional analysis " (Deng Ganchun, Zeng Changmin,
Tian Binqiang etc., the extraction of Ginkgo oil and fatty acid compositional analysis Chinese oil, 2007,32 (10): 76-79) in disclose will be new
Fresh ginkgo shelling crushes after freeze-drying, and supercritical fluid extraction is up to Ginkgo oil.Contain 16 kinds of fat in gained Ginkgo oil
Acid, wherein unsaturated fatty acid accounts for the 91.4% of total fatty acid content, and the content of linoleic plus oleic acid accounts for 75.4%.
Li Yingxia, Zhou Shan, Zhong Ling, Wu Yan, Ge Fahuan are in " Response Surface Method optimization supercritical CO2Fluid extraction Ginkgo oil
Technical study and its constituent analysis " (Li Yingxia, Zhou Shan, Zhong Ling, Wu Yan, Ge Fahuan Response Surface Method optimize supercritical CO 2
The technical study and its constituent analysis Chinese medicine of fluid extraction Ginkgo oil, 2011,34 (2): 298-301) in will crush after gingko
Loaded in extraction kettle, extraction kettle, separating still I, separating still II are respectively heated, cold refrigeration is opened simultaneously, when temperature reaches
It boosts after to sets requirement, after reaching selected pressure, closes CO2Gas cylinder starts the cycle over extraction, and keeps constant temperature and pressure, reaches
After the selected time, is exported from separating still I and collect product, obtain Ginkgo oil.Supercritical CO2Extract the optimised process of Ginkgo oil
Are as follows: extracting pressure 29.01Mpa, 40.38 DEG C of extraction temperature, extraction time 120min, yield 4.46%；Insatiable hunger in Ginkgo oil
It is 76.8% with content of fatty acid, main component 8,11- octadecadienoic acid (35.09%), 9- octadecenoic acid
(16.49%), vaccenic acid (15.97%).
Chen Xijuan, Wang Chengzhang, Chen Hongxia, Ye Jianzhong are in " extraction process and its chemical constitution study of Ginkgo oil " (Chen Xi
Juan, Wang Chengzhang, Chen Hongxia, the extraction process and its northwest chemical constitution study Botany Gazette of Ye Jianzhong Ginkgo oil, 2010,30
(4): 838-843 it discloses in) using supercritical CO2Fluid extraction Ginkgo oil, and petroleum ether is added as entrainer, best work
Skill condition are as follows: 40 DEG C of temperature, pressure 20MPa, flow velocity 15L/h, time 3h, oil yield is in different cultivars gingko dry powder
3.6%-7.11%.17 kinds of chemical components are identified from supercritical extract Ginkgo oil, wherein unsaturated fatty acid accounts for 85.4%；
Unsaturated fatty acid is based on 16,18 carbon.
Application publication number CN104560403A discloses " a kind of gingko essential oil and preparation method thereof ", and gingko dry powder is passed through
95% ethyl alcohol extracts, and filters, and is concentrated under reduced pressure, and molecular distillation obtains gingko essential oil, but the object that undisclosed gingko essential oil specifically includes
Matter and quality evaluating method.
In gingko essential oil other than containing unsaturated fatty acid, also recklessly containing active constituent ginkgoterpene lactone, flavones and class
Radish element substance.Existing gingko essential oil mostly uses greatly supercritical CO2Fluid extraction mode, non-broken wall crushes before supercritical extract,
Recovery rate is low, and without a series of extraction in front with enrichment only with molecular distillation, treating capacity is small, and production efficiency is low, and impurity contains
Amount is high.The relatively common vegetable edible oil oil content of ginkgo nut is low, there is no efficient, energy conservation and environmental protection, green manufacturing, integrated innovation at present
Technology commercialization produces ginkgo oil, more has no new technology use in conjunction, wherein unsaturated fatty acid, active constituent are silver-colored for Extraction and enrichment
Apricot terpene lactone and flavones, xanthophyll, β-and alpha-carotene carotenoid are not known where to begin more.Ginkgo oil noxious material ginkgoic acid
< 1ppm is lower than United States Pharmacopeia and European Pharmacopoeia≤5ppm and Chinese Pharmacopoeia≤10ppm, also has not been reported.
Summary of the invention
In order to solve current gingko essential oil only with supercritical CO2Fluid extraction, can not Sync enrichment unsaturated fatty acid,
The problem of Terpene lactones, flavones, xanthophyll, β-and alpha-carotene carotenoid, the object of the present invention is to provide one kind
The extracting method of ginkgo essential oil, unsaturated fatty acid accounts for total fatty acids > 92%, total in the ginkgo essential oil obtained using this method
Flavones > 0.10%, contain Bilobalide and Ginkgolide A. B. C, total terpene lactone > 0.02%, contain xanthophyll, β-and α-
Carrotene, 1 ㎎ of carotenoid total amount >/100g.Noxious material ginkgoic acid < 1ppm is lower than 2015 USP 38 of United States Pharmacopeia
Version, 2015 editions≤10ppm of European Pharmacopoeia (UP 2014 editions)≤5ppm and Chinese Pharmacopoeia.
To achieve the goals above, the present invention adopts the following technical scheme: a kind of extracting method of ginkgo essential oil, including such as
Lower step:
S1 after ginkgo nut is mixed with water, carries out ultrasonic vibration and cyclonic separation processing, obtains food containing gingko almond particle；
S2, the ginkgo nut particle that S1 is obtained carry out supercritical fluid extraction processing, obtain ginkgo nut crude oil；
S2 is obtained the progress molecular distillation of ginkgo nut crude oil and obtains ginkgo essential oil by S3.
Using the above scheme, ginkgo nut ginkgo plumule and ginkgo nut particle after ultrasonic vibration is detached from, and is made in cyclonic separation
Under, ginkgo plumule and ginkgo nut particle are thoroughly separated, and ginkgo nut particle successively carries out supercritical fluid extraction and molecular distillation
Processing obtains ginkgo essential oil, and unsaturated fatty acid accounts for total fatty acids > 92%, general flavone > 0.10%, contains in ginkgo essential oil
Total terpene lactone > 0.02%, Bilobalide and Ginkgolide A. B. C contain xanthophyll, β-and alpha-carotene, carotenoid
1 ㎎ of total amount >/100g.Noxious material ginkgoic acid < 1ppm is lower than 2015 USP of United States Pharmacopeia 38 editions, European Pharmacopoeia (UP
2014 editions) 2015 editions≤10ppm of≤5ppm and Chinese Pharmacopoeia.
It wherein, further include that crush processing step is carried out to ginkgo nut in the S1 before ginkgo nut is mixed with water.
Ginkgo nut exposes ginkgo plumule sufficiently through crusher, endotesta and mesosperm rupture, plumule after ultrasonic vibration
It quickly loosens and separates with fat deposit, separation rate reaches 60% or more, and endotesta and mesosperm separate.
Preferably, the crush processing step treated ginkgo nut granularity is 10-40 mesh.
Using the above scheme, ginkgo plumule sufficiently exposes, and is convenient for ultrasonic vibration step by ginkgo plumule and ginkgo nut particle
It is detached from.
Wherein, the mixed proportion of ginkgo nut and water is 1:6-1:15 in the S1.
Preferably, the frequency of ultrasonic vibration is 45-80HZ in the S1, and the time of ultrasonic vibration is 20-50 minutes.
Using the above scheme, ginkgo plumule is sufficiently disengaged from gingko nut.
Wherein, separation equipment is cyclone separator in the S1.
Using cyclone separator eddy flow, eddy flow is by high-pressure delivery material, and the continuous tube wall that hits forces plumule and fat
Separation, final separation rate reach 95% or more.Due to density contrast between mesosperm, endotesta, plumule and ginkgo endosperm paste, trip
From plumule overflowed by overflow port, ginkgo endosperm paste is discharged from lower part, and successively upper end is discharged for ginkgo nut endotesta and mesosperm,
Achieve the effect that thoroughly separated.
Wherein, in S2 before supercritical fluid extraction processing, further includes: vacuum drying step.
The water content of food containing gingko almond particle reduces the influence that moisture handles supercritical extract less than 5% after drying.
Wherein, in S2 before supercritical fluid extraction processing, further includes: crush, screening step.
The granularity control of ginkgo nut particle puts into 200 purposes between 180-220 mesh, then by the material of collection after crushing
It is sieved in rotation sub-sieve, ginkgo nut particle uniform particle diameter, treatment effect is stablized.
Wherein, in S2 before supercritical fluid extraction processing, further includes: air-flow broken wall pulverising step.
By air-flow broken wall pulverising step, the granularity of food containing gingko almond powder is 1250-3000 mesh, and ginkgo nut cell wall is abundant
It destroys, improves oil yield.
Wherein, the equipment that air-flow broken wall crushes is airslide disintegrating mill.
Wherein, in S2 after air-flow broken wall pulverising step, further includes: mixing and granulation step.
By air-flow broken wall pulverising step, the undersized of food containing gingko almond powder, in supercritical fluid extraction, food containing gingko almond
Powder is pressed into pie, CO2Mobility be obstructed, influence effect of extracting；By pelletizing after mixing, granularity control is in 20-40 mesh, extraction
CO when taking2Good fluidity.
It wherein, further include that adhesive step is added before mixing and granulation step.
The adhesive be starch, pre-gel starch, polyvinylpyrrolidone, methylcellulose, sodium carboxymethylcellulose,
One of ethyl cellulose, polyvinyl alcohol or a variety of mixing.
Wherein, in S2 before supercritical fluid extraction processing, further includes: microwave drying sterilization step.
After dry sterilization, for the moisture content of material less than 5%, total plate count is less than 1000cfu/g, obtains after avoiding processing
Ginkgo essential oil generate spoilage problem, guarantee ginkgo essential oil edible safety.
Wherein, between supercritical fluid extraction processing and molecular distillation, further includes: solvent recovery and deodorization processing step
Suddenly.
Crude oil after supercritical extract is added in stage falling-film formula Vacuum film evaporation device and carries out solvent recovery, it will be silver-colored
Apricot fruit crude oil is concentrated, and then the ginkgo nut crude oil after concentration is added in two-stage scraper type Vacuum film evaporation device and is carried out
Vacuum deodorization obtains ginkgo nut first oil.
Deodorization treated ginkgo nut first oil odorless, user's embodiment degree are more preferable.
Wherein, between supercritical fluid extraction processing and molecular distillation, further includes: refrigerated centrifuge step.
Wherein, between supercritical fluid extraction processing and molecular distillation, further includes: vacuum filtration step.
Refrigerated centrifuge and vacuum filtration step are removal steps, improve the purity of ginkgo essential oil.
It preferably, further include that entrainer step is added before supercritical fluid extraction in the S4.
The entrainer is selected from methanol, ethyl alcohol, acetone or ethyl acetate.
The addition of entrainer is greater than the extraction of the flavones and terpene lactone of grease convenient for polarity.
Preferably, in the S4 supercritical fluid extraction process conditions: extraction kettle pressure 30-35MPa, extract kettle temperature
25-45 DEG C, separating still pressure 6-10MPa of degree, 40-65 DEG C of separating still temperature, extraction time 1.5-3h.
Ginkgo nut is obtained by ultrasonic vibration and cyclonic separation processing, supercritical fluid extraction processing and molecular distillation processing
Ginkgo essential oil is obtained, wherein unsaturated fatty acid accounts for total fatty acids > 92%, general flavone > 0.10%, contains gingko in ginkgo essential oil
Total terpene lactone > 0.02%, lactone and Ginkgolide A. B. C contain xanthophyll, β-and alpha-carotene, carotenoid total amount
1 ㎎ of >/100g.Noxious material ginkgoic acid < 1ppm is lower than 2015 USP of United States Pharmacopeia 38 editions, European Pharmacopoeia (UP 2014 editions)
2015 editions≤10ppm of≤5ppm and Chinese Pharmacopoeia.Crush processing step is added before ultrasonic vibration processing, and overcritical
Vacuum drying step is added before fluid extraction processing, crushes, screening step, air-flow broken wall pulverising step, mixing and granulation step
Suddenly, only increase the oil yield of ginkgo nut, improve extraction efficiency, recklessly to unsaturated fatty acid, general flavone, total terpene lactone, class
Radish element total amount and the content of noxious material ginkgoic acid are unaffected；Microwave drying is added before supercritical fluid extraction processing
Sterilization steps guarantee sterilization effect with supercritical fluid extraction step collective effect, avoid the corruption of ginkgo essential oil, improve food
Use safety；Supercritical fluid extraction processing molecular distillation between be added solvent recovery and deodorization processing step, freeze from
Heart step and vacuum filtration step, for improving the purity of ginkgo essential oil.
Compared with prior art, the present invention realize the utility model has the advantages that in the extracted ginkgo essential oil of extracting method of the present invention
Unsaturated fatty acid accounts for total fatty acids > 92%, general flavone > 0.10%, containing Bilobalide and Ginkgolide A. B. C, total terpene
Class lactone > 0.02%, contain xanthophyll, β-and alpha-carotene, 1 ㎎ of carotenoid total amount >/100g.Noxious material ginkgo
Sour < 1ppm is lower than 2015 USP of United States Pharmacopeia 38 editions, European Pharmacopoeia (UP 2014 editions)≤5ppm and Chinese Pharmacopoeia 2015 editions
≤10ppm；Oil yield of the present invention after supercritical extract step is stablized 7% or so.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, present invention be described in more detail:
Fig. 1 is the flow chart of ginkgo method of extraction of essential oil of the present invention.
Specific embodiment
As the extracting method of Fig. 1, ginkgo essential oil include the following steps:
One, destruction step
It opens crusher to put into ginkgo peaberry in crusher after its normal operation, controls the speed of crusher
Between -3500/ minute 2900/ minute, so that the particle size after cracking of food containing gingko almond, between 10-40 mesh, ginkgo plumule is sufficiently sudden and violent
It is spare to collect the food containing gingko almond particle being crushed for dew.
Two, ultrasonic vibration step
The food containing gingko almond particle being crushed is mixed according to the ratio of 1:6-1:15 with water, put into ultrasonator into
Row concussion, oscillation frequency 45-80HZ, concussion time are 20-50 minutes, are detached from ginkgo plumule and food containing gingko almond particle, will
The good material of ultrasonic vibration is fitted into spare in rustless steel container.
Three, eddy flow takes off plumule step
The good food containing gingko almond particle of ultrasonic vibration is squeezed into cyclone separator with 0.1Mpa, adjusts pressure 0.3Mpa-
The separation of 1.0Mpa progress plumule.Lightweight collects ginkgo plumule from the upper end overflow port of cyclone separator, and heavy is in eddy flow point
Lower end discharge outlet from device collects food containing gingko almond particle, drains drying for standby after purified water.
Four, vacuum drying step
The food containing gingko almond particle for removing plumule is packed into stainless steel plate, is put into vacuum desiccator and is dried, make silver
The water content of apricot kernel particle is less than 5%.
Five, it crushes, screening step
Food containing gingko almond particle to be put into pulverizer and is crushed, the granularity of crushing controls between 180-220 mesh, then
The material of collection is put into the rotation sub-sieve of 200 mesh and sieved, the food containing gingko almond powder sieved collected spare.
Six, air-flow broken wall pulverising step
The food containing gingko almond powder sieved is put into progress broken wall crushing in airslide disintegrating mill, makes the granularity of food containing gingko almond powder
For 1250-3000 mesh, it is spare to collect the good food containing gingko almond powder of broken wall.
Seven, mixing and granulation step
The good food containing gingko almond powder of broken wall is put into mixing machine, suitable adhesive is added and is sufficiently mixed, then
The material mixed is put into granulator and is pelletized, granularity is 20-40 mesh, and the particle made is fitted into stainless steel disc
It is spare.
Eight, microwave drying sterilization step
The stainless steel disc for filling food containing gingko almond particle is put into microwave drying sterilization device, sterilizing is dried, makes material
Moisture content is less than 5%；Total plate count is less than 1000cfu/g.
Nine, supercritical CO2Extraction step
Ginkgo fruit granule is fitted into the charging basket of extractor, charged charging basket is mounted in extraction kettle, gland is covered
And upper plug head, technological parameter is set；Start to extract, supercritical extraction process parameter: extraction kettle pressure is 25Mpa-35Mpa, extraction
Taking kettle temperature degree is 25 DEG C -45 DEG C, and separating still pressure is 5Mpa-10Mpa, and separating still temperature is 40 DEG C -65 DEG C, and extraction time is
1.5-3 hours, after extraction, it is spare that ginkgo nut crude oil is collected from separating still.
Supercritical fluid extraction (supercritical fluid extraction, SFE) technology refers to gas compression
To more than critical point, supercriticality is made up to, thus be allowed to possess the viscosity of gas and the density of liquid simultaneously, it is this super
Critical state can greatly increase gas to the solvability of solute.And the gas in a supercritical state when changing pressure and temperature
Know from experience and restores gaseous state, and the solute wherein dissolved will parse.
Supercritical fluid extraction feature:
(1) supercritical fluid extraction rate is high, and rate of extraction is fast, and technological parameter is easy to control, and can guarantee product quality.
(2) extraction and separation are combined into one
Pressure declines so that fluid rapidly becomes two-phase (gas-liquid separation) with extract and separates immediately, and there is no materials
Phase transition process is not necessarily to recycling design, can be recycled after solvent is pressurized, easy to operate, consumes less, save the cost.
(3) it is extracted under cryogenic conditions
Supercritical fluid extraction usually carries out at a lower temperature, can be effectively prevented the oxidation and ease of heat-sensitive ingredients
It dissipates, the separation and Extraction strong to heat sensitivity particularly suitable for those, easy to oxidize for decomposing ingredient.
(4) there is no residual solvent
Gas under supercritical carbon dioxide fluid normality, it is nontoxic separated with extraction component after, absolutely not solvent is residual
It stays, efficiently solves the problem of solvent residual of traditional extraction process.
(5) selectivity and solubility property are good, extract complete
The solvability of fluid and the size of its density are related, and temperature, the minor change of pressure all can cause fluid close
Degree is widely varied, and correspondingly shows as the variation of solubility.Therefore, it can use pressure, the variation of temperature is realized
Extraction and isolated process.By selecting suitable extractant and operating condition, can selectively effective component extracting, and mention
Purity is high is taken, subsequent separation is convenient for, product yield improves.
(6) extraction rate is fast, with short production cycle
Supercritical CO_2 extraction (dynamic) recycles at the beginning, and separation just starts to carry out.General extract just has ingredient point for 10 minutes
It isolates, can extract completely within 2~4 hours or so.Meanwhile it is not required to concentration step.
(7) separating technology process is simple.
Supercritical extract is only made of extractor and separator two parts, does not need solvent reclaimer, easy to operate, section
Labour and a large amount of organic solvents are saved, pollution is reduced.
(8) supercritical CO 2 also has anti-oxidant, sterilization functions, advantageously ensures that and improve product quality.
(9) industrialized production can be used for.
Before starting extraction, entrainer can be added into extraction kettle, the entrainer that can choose is methanol, ethyl alcohol, third
Ketone or ethyl acetate.
Ten, solvent recovery and deodorization processing step
Crude oil after supercritical extract is added in stage falling-film formula Vacuum film evaporation device and carries out solvent recovery, it will be silver-colored
Apricot is concentrated except crude oil, and then the ginkgo nut crude oil after concentration is added in two-stage scraper type Vacuum film evaporation device and is carried out
It is spare to obtain ginkgo nut first oil from the discharge outlet of scraper-type Vacuum film evaporation device for vacuum deodorization.
11, refrigerated centrifuge step
The ginkgo nut first oil of acquisition is subjected to refrigerated centrifuge, to separate the residue in first oil, by ginkgo nut after refrigerated centrifuge
First oil collection, which is fitted into stainless steel oil tank, to be sent to next procedure.
12, vacuum filtration step
Ginkgo nut first oil is subjected to vacuum filter, the insoluble impurities in first oil is completely removed, after vacuum filter
Ginkgo nut first oil be fitted into stainless steel oil tank and send to next procedure.
13, molecular distillation step
Ginkgo nut first oil after vacuum filter is subjected to molecular distillation, running parameter: vacuum degree 10-3- 5Pa, evaporating surface turn
Fast 500r/min-2000r/min, -100 DEG C of evaporating surface temperature 60 C；0 DEG C -10 DEG C of cryosurface temperature.Through the feed liquid on rotor point
It is continuously and uniformly distributed on heating surface by cloth device, and feed liquid is spread to one layer of liquid film very thin, in turbulence-like by blade applicator immediately,
And it spirally advances downwardly.In the process, the light molecule escaped from heating surface, through too short route and almost without touching
It hits and is condensed into liquid on built-in condenser of arriving, and flowed down along condenser tube, the discharge nozzle by being located at base of evaporator is discharged；It is residual
Liquid, that is, weight molecule is collected in the circular channel under heating zone, then is flowed out in the discharge nozzle for passing through side.To be refined
Ginkgo essential oil after molecular distillation is fitted into stainless steel oil tank and send to procedures such as bottlings by ginkgo essential oil.
Molecular distillation (also referred to as short-path distillation) is the continuous still that (0.1~100Pa) is carried out under a high vacuum.It is one
The special liquid-liquid separation technology of kind, its essence is the evaporation processes of molecule.
Molecular distillation can be widely used in the isolation technics of industrialized production, and can solve wide variety of conventional distillation technique cannot
It solves the problems, such as.Molecular distillation can operate under high vacuum degree, and the difference of its foundation molecular tools can make
Liquid far below its boiling point at a temperature of be isolated, especially suitable for higher boiling, thermal sensitivity and oxidizable compound
Separation.Again because the technology has vapo(u)rizing temperature lower than the boiling point of material, distillation pressure is low, heated time is short, separation degree is high
The features such as, thus the separation costs of high boiler material can be substantially reduced, admirably protect the quality of heat sensitive material.This technology
It is widely used to the extraction of natural health-care products, the constraint of chemical treatment method can be got rid of, really maintains pure natural characteristic,
The quality of health product is stepped to step on a new stage.
The characteristics of molecular distillation technique
From the point of view of the form that the technical principle and equipment of molecular distillation design, molecular distillation technique and conventional distil-lation or decompression
Distillation technique is compared, and is a kind of mild isolation technics, it has the characteristics that the following.
(1) distillation pressure is low, and the high conventional distil-lation device of vacuum degree is since there are the resistances of filler or column plate, so system is very
Hardly possible obtains higher vacuum degree, is generally only capable of reaching 5kPa or so.And molecular distillation apparatus is pressed since internal structure is fairly simple
It is strong minimum, so easily obtaining relatively high vacuum degree (0.1~100Pa), it is more advantageous to the separation for carrying out material.
(2) the low conventional distil-lation of vapo(u)rizing temperature is the operation carried out at a temperature of material boiling point, and molecular distillation is using not
Mean free path after congener molecule evolution liquid level different property realizes separation, so can be far below boiling point
At a temperature of operated, material does not need to boil, operation temperature than conventional vacuum distillation can be 50~100 DEG C low.It can be seen that
Molecular distillation technique is more advantageous to energy saving, the separation of especially some higher boilings, heat sensitive material, is more suitable for using this
Technology.
It can be obtained from two above feature, molecular distillation is usually to carry out in the case where being far below conventional distil-lation temperature
Operation.Due to being operated under fluidized state, evaporating temperature compares molecular distillation for generally conventional vacuum distillation or rectification under vacuum
It is much higher.In addition the resistance of its column plate or filler, it is more much bigger than molecular distillation, it is obtained so its operation temperature is higher than molecular distillation
It is more.If operation temperature of certain mixture in vacuum distillation is 260 DEG C, and same mixture only needs 150 in molecular distillation
℃。
(3) since molecular distillation vacuum degree is high, low operation temperature and heated time is short, for higher boiling and thermal sensitivity and easily
The separation of oxidation material is able to achieve the physical process that traditional separation method cannot achieve, therefore, in point of some high value materials
It is widely used as the means of deodorization, decoloration and purification from, and selectively steams target product, removes other impurity, very
It protects separated object matter not contaminated well and encroaches on, guarantee the natural quality of material.
Material heated time it is short by molecular distillation principle it is found that the required distance between the liquid level and cryosurface that are heated is less than
The mean free path of light molecule, and the light molecule escaped by liquid level, almost just reach cryosurface, so heated time without collision
It is very short.In addition, mixing liquid is in film-form, keep the area of liquid level and heating surface almost equal, such material is in distillation process
Heated time just becomes shorter.For vacuum distillation, heated time is 1 hour, and molecular distillation only needs more than ten seconds.
For conventional distil-lation, condensation is escaped into from boiling liquid level by separation component and is distillated, since the distance walked is longer,
So heated time is longer；And molecular distillation condenses walked path and wants small since gaseous molecular from liquid level escapes into cryosurface
In its mean free path, distance is shorter, so the time that material is in gaseous state this heating status is just shorter, is typically only 0.05
~15 seconds.
(4) distillation of separation degree more macromolecule is usually used to separation conventional distil-lation and is not easy separated substance (do not include same point
The separation of isomers).And for the substance that can be separated with two methods, the separation degree of molecular distillation is higher, and separates
Degree is related with relative volatility.
The present invention by repeatedly experiment discovery, when crusher speed be 2900/ minute, the use of food containing gingko almond particle and water
Amount ratio is 1:9, oscillation frequency 60HZ, and the concussion time is 30 minutes, and the pressure of cyclone separator is 0.8Mpa, air-flow broken wall
Smashed granularity is 2000 mesh, supercritical CO2Extraction kettle pressure is 32Mpa when extraction, and extraction kettle temperature is 35 DEG C, separating still
Pressure is 6Mpa, and separating still temperature is 55 DEG C, and extraction time is 2.5 hours, can greatly shorten extraction time, improve extraction
Efficiency.
Embodiment 1
4 tons of ginkgo nut are taken, cleans, drains.It is put into crusher, is adjusted crusher 2900/ minute with suitable speed,
Particle size after cracking is controlled in 10 mesh, and the food containing gingko almond particle being crushed is mixed according to 1 to 15 with purified water, ultrasonic vibration is put into
It is shaken, frequency 70-80HZ concussion processing 30 minutes, the good food containing gingko almond particle of ultrasonic vibration is squeezed into 0.1Mpa in device
In 5 grades of cyclone separators, the separation that pressure 0.3Mpa carries out plumule is adjusted.Heavy is received in the lower end discharge outlet of cyclone separator
Collect food containing gingko almond, drains purified water, be dried under vacuum to water content less than 5%.Dry food containing gingko almond particle is put into pulverizer
In crushed, sieved in the sub-sieve of 200 mesh, the food containing gingko almond powder sieved put into airslide disintegrating mill and is carried out
Broken wall crushes, and grinding particle size is 1250 mesh, and suitable adhesive is added and is uniformly mixed, puts into granulator and pelletizes, receives
Collect 20 mesh to 40 mesh particles, microwave drying sterilization is fitted into the charging basket of supercritical extract device, extraction kettle pressure: 30Mpa, extraction
Kettle temperature degree: 25 DEG C, separating still pressure: 8Mpa, separating still temperature: 40 DEG C, entrainer methanol, extraction time: 1.5 hours, extraction
After, ginkgo nut crude oil, oil yield 6.62% are collected from separating still.Crude oil after extraction is added to stage falling-film formula vacuum
Recycling design in thin film evaporator is then added in two-stage scraper type Vacuum film evaporation device and carries out vacuum deodorization, from discharging
Ginkgo nut first oil is collected at mouthful.Ginkgo nut crude oil is carried out molecular distillation, running parameter is arranged: is true by refrigerated centrifuge, vacuum filter
Reciprocal of duty cycle 10-1Pa,；Evaporating surface revolving speed 1500r/min；Evaporating surface temperature 60 C；0 DEG C of cryosurface temperature, the ginkgo essence refined
Oil, oil yield 4.81%.Ginkgo essential oil after molecular distillation is fitted into stainless steel oil tank and is sent to procedures such as bottlings.
Embodiment 2
2 tons of ginkgo nut are taken, cleans, drains.It is put into crusher, is adjusted crusher 3200/ minute with suitable speed,
Particle size after cracking is controlled in 10 mesh, and the food containing gingko almond particle being crushed is mixed according to 1 to 9 with purified water, ultrasonic vibration is put into
It is shaken in device, frequency 60HZ concussion processing 30 minutes, the good food containing gingko almond particle of ultrasonic vibration is squeezed into 4 grades with 0.1Mpa
In cyclone separator, the separation that pressure 0.8Mpa carries out plumule is adjusted.Heavy is collected in the lower end discharge outlet of cyclone separator
Food containing gingko almond drains purified water, is dried under vacuum to water content less than 5%.Dry food containing gingko almond particle is put into pulverizer
It is crushed, is sieved in the sub-sieve of 200 mesh, the food containing gingko almond powder sieved is put into airslide disintegrating mill and is carried out brokenly
Wall crushes, and grinding particle size is 2000 mesh, and suitable adhesive is added and is uniformly mixed, puts into granulator and pelletizes, collects
20 mesh to 40 mesh particles, microwave drying sterilization is fitted into the charging basket of supercritical extract device, extraction kettle pressure: 32Mpa, extraction kettle
Temperature: 35 DEG C, separating still pressure: 5Mpa, separating still temperature: 55 DEG C, entrainer ethyl acetate, extraction time: 2.0 hours, extraction
After taking, ginkgo nut crude oil, oil yield 7.19% are collected from separating still.Extraction crude oil is added to stage falling-film formula vacuum
Recycling design in thin film evaporator is then added in two-stage scraper type Vacuum film evaporation device and carries out vacuum deodorization, from discharging
Ginkgo nut first oil is collected at mouthful.Ginkgo nut crude oil is carried out molecular distillation, running parameter is arranged: is true by refrigerated centrifuge, vacuum filter
Reciprocal of duty cycle 10-2Pa；Evaporating surface revolving speed 1000r/min；100 DEG C of evaporating surface temperature；2 DEG C of cryosurface temperature.The ginkgo essence refined
Oil, oil yield 5.12%.Ginkgo essential oil after molecular distillation is fitted into stainless steel oil tank and is sent to procedures such as bottlings.
Embodiment 3
5 tons of ginkgo nut are taken, cleans, drains.It is put into crusher, is adjusted crusher 3500/ minute with suitable speed,
Particle size after cracking is controlled in 30-40 mesh, and the food containing gingko almond particle being crushed is mixed according to 1 to 6 with purified water, ultrasonic shake is put into
It swings in device and is shaken, frequency 45-50HZ concussion processing 20 minutes, the good food containing gingko almond particle of ultrasonic vibration is beaten with 0.1Mpa
Enter in 6 grades of cyclone separators, adjusts the separation that pressure 1.0Mpa carries out plumule.Lower end discharge outlet of the heavy in cyclone separator
Food containing gingko almond is collected, purified water is drained, is dried under vacuum to water content less than 5%.Dry food containing gingko almond particle is put into crushing
Crushed in machine, sieved in the sub-sieve of 200 mesh, by the food containing gingko almond powder sieved put into airslide disintegrating mill into
Row broken wall crushes, and grinding particle size is 3000 mesh, and suitable adhesive is added and is uniformly mixed, puts into granulator and pelletizes,
20 mesh are collected to 40 mesh particles, microwave drying sterilization is fitted into the charging basket of supercritical extract device, extraction kettle pressure: 25Mpa, extraction
Take kettle temperature degree: 45 DEG C, separating still pressure: 10Mpa, separating still temperature: 65 DEG C, extraction time: entrainer ethyl alcohol 3 hours, extracts
After, ginkgo nut crude oil, oil yield 7.53% are collected from separating still.It is thin that extraction crude oil is added to stage falling-film formula vacuum
Recycling design in film evaporator is then added in two-stage scraper type Vacuum film evaporation device and carries out vacuum deodorization, from discharge port
Collect ginkgo nut first oil in place.Ginkgo nut crude oil is carried out molecular distillation, running parameter: vacuum is arranged by refrigerated centrifuge, vacuum filter
Degree 10-3Pa；Evaporating surface revolving speed 500r/min；80 DEG C of evaporating surface temperature；10 DEG C of cryosurface temperature.The ginkgo essential oil refined,
Oil yield 5.31%.Ginkgo essential oil after molecular distillation is fitted into stainless steel oil tank and is sent to procedures such as bottlings.
Embodiment 4
GC-MS method carries out Analysis of Fatty Acids Composition in ginkgo essential oil
Specific test method is referring to " fatty acid compositional analysis in Linseed oil " and " Response Surface Method optimizes supercritical CO 2
(fatty acid compositional analysis drug divides the technical study and its constituent analysis of fluid extraction Ginkgo oil " in Wang Yingqiang Linseed oil
Analyse magazine, 1998,18 (3): 176.；Li Yingxia, Zhou Shan, Zhong Ling, Wu Yan, Ge Fahuan Response Surface Method optimize SCF-CO 2
Body extracts the technical study and its constituent analysis Chinese medicine of Ginkgo oil, 2011,34 (2): 298-301.).
It takes 0.5g ginkgo raw sample/purification ginkgo essential oil to have in plug round-bottomed flask in 25mL, 0.5molL is added-1Hydrogen
The methanol solution 2mL of potassium oxide, shakes up, and is placed in saponification 30min (oil droplet completely disappears) in 60 DEG C of water-baths, is added 14% after cooling
The methanol solution 2mL of boron trifluoride, shakes up, and in being esterified 6min in 60 DEG C of water-baths, cooling adds n-hexane and saturated sodium-chloride water-soluble
Each 2mL of liquid, shakes up, and hierarchical is clear, takes supernatant as GC/MS Analysis sample.
Instrument: PE Clarus 680/SQ8T GCMS,
Chromatographic column: 0.25 μm of PE Elite-530m 0.32mm,
Column temperature:, keeping 5min by 60 DEG C of initial temperature, is warming up to 240 DEG C with the rate of 3 DEG C/min, keeps 25min,
Injector temperature: 220 DEG C,
Detector temperature: 280 DEG C,
MS interface temperature: 280 DEG C,
Ion source temperature: 230 DEG C,
Carrier gas: high-purity helium,
Flow rate of carrier gas: 20psi constant voltage mode,
Split ratio: 100:1,
Sample volume: 0.1 μ L.
A variety of insatiable hungers contained in the ginkgo essential oil that calculating supercritical extract ginkgo crude oil and molecular distillation are refined
The percentage of total fatty acids is accounted for fatty acid, the results are shown in Table 1.
Table 1
Embodiment 5
The measurement of general flavone in ginkgo essential oil
Measuring method is referring to " chemical constitution study of the content of general flavone and its grease in gingko " (National Pharmacopeia committee member
Meeting Pharmacopoeia of People's Republic of China: one Beijing of version in 2015: China Medical Science Press, 2015:417.；Katrina Leung,
Wang Chengzhang, Gao Caixia wait the content of general flavone and its chemical constitution study [J] biomass chemical engineering of grease in gingko,
2006,40(6):6-8)。
Agilent 1100 Infinity liquid chromatograph (1100 quaternary pump of Agilent, DAD detector, Agilent
1100 autosamplers, Agilent Chemstation software, Agilent Co., Ltd, the U.S.)；
Agilent Eclipse Plus C18 chromatographic column, (column length 150mm, column internal diameter 4.6mm, partial size are 5 μm).
Quercetin reference substance (Chengdu Rui Fensi Biotechnology Co., Ltd, purity > 98%),
Kaempferol reference substance (Chengdu Rui Fensi Biotechnology Co., Ltd, purity > 98%),
Isorhamnetin reference substance (Nat'l Pharmaceutical & Biological Products Control Institute).
With -0.4% phosphoric acid solution of methanol (50:50) for mobile phase；Detection wavelength is 360mn.
The preparation of reference substance solution: taking Quercetin reference substance appropriate, accurately weighed, adds methanol that every lmL is made containing 30mg's
Solution to get.
The preparation of test solution: taking ginkgo raw sample/purification ginkgo essential oil about 2g, accurately weighed, adds methanol -25%
The mixed solution 25ml of hydrochloric acid solution (4:1) sets and is heated to reflux in water-bath 30 minutes, is rapidly cooled to room temperature, is transferred to 50ml
In measuring bottle, with methanol dilution to scale, shake up, filter, take filtrate to get.
Measuring method: accurate absorption reference substance solution and each 10 μ l of test solution respectively, injection liquid chromatograph, measurement,
It is control with the peak area of Quercetin reference substance, the corresponding correction factor of according to the form below calculates Quercetin, Kaempferide and different respectively
The content of rhamnetin, with the relative retention time of ingredient chromatographic peak to be measured and Quercetin chromatographic peak determine Quercetin, Kaempferide and
The peak position of Isorhamnetin, relative retention time should be within the scope of specified value taxis 5% (if relative retention time deviation is more than
5%, then should be subject to and be confirmed accordingly by substitute reference substance) to get.Shown in relative retention time and correction factor (F) table 2.
Table 2
Total flavonoids content=(quercetin content+kaempferia galanga cellulose content+Isorhamnetin content) × 2.51
Measure supercritical extract ginkgo crude oil and ginkgo essential oil that molecular distillation is refined in total flavonoids content such as
Shown in table 3.
Table 3
| Total flavonoids/% in supercritical extract ginkgo crude oil | Total flavonoids/% in the ginkgo essential oil of purification | |
| Embodiment one | 0.0836 | 0.1199 |
| Embodiment two | 0.0782 | 0.1009 |
| Embodiment three | 0.0725 | 0.1204 |
Embodiment 6
The measurement of total terpene lactone in ginkgo essential oil
Measuring method is referring to the finger-print of gingko benevolence terpene lactone ingredient " study " (Chinese in Chinese Pharmacopoeia Commission
People republic pharmacopeia: one Beijing of version in 2015: China Medical Science Press, 2015:416-417.；Luo Man, Bao Jiake,
Xiong Huilin waits the finger-print of gingko benevolence terpene lactone ingredient to study Chinese patent drug, 2011,33 (9): 1465-1469.；Zhang Qun
Group, Li Huifen, Zhang Xuelan, wait .HPLC_ELSD method and meanwhile measure in different sources gingko medicinal material in 4 kinds of terpene lactones ingredient at
Medicine, 2016,38 (1): 133-136.).
Agilent 1100 Infinity liquid chromatograph (1100 quaternary pump of Agilent, DAD detector, Agilent
1100 autosamplers, Agilent Chemstation software, Agilent Co., Ltd, the U.S.)；
Agilent Eclipse Plus C18 chromatographic column, (column length 150mm, column internal diameter 4.6mm, partial size are 5 μm)；
Ginkalide A reference substance (Nat'l Pharmaceutical & Biological Products Control Institute),
Ginkolide B reference substance (Nat'l Pharmaceutical & Biological Products Control Institute),
Ginkalide C reference substance (Nat'l Pharmaceutical & Biological Products Control Institute),
Bilobalide reference substance (Nat'l Pharmaceutical & Biological Products Control Institute).
With normal propyl alcohol-tetrahydrofuran-water (1:15:84) for mobile phase；It is detected with evaporative light scattering detector.
The preparation of reference extract solution: taking ginkgo biloba leaf total terpene lactone reference extract appropriate, accurately weighed, and methanol is added to be made
Solution of every lmL containing 2.5mg to get.
The preparation of test solution: taking ginkgo raw sample/purification ginkgo essential oil about 2g, accurately weighed, adds water 10ml, sets
Warm makes to dissolve in water-bath, and 2% hydrochloric acid solution 2 is added to drip, and is shaken with ethyl acetate and extracts 4 times (15ml, 10ml, 10ml, 10ml),
Combined extract is washed with 5% sodium acetate solution 20ml, is divided and is taken sodium acetate liquid, then is washed with ethyl acetate 10ml, and acetic acid is merged
Ethyl ester extracting solution and cleaning solution are washed with water 2 times, each 20ml, and point water intaking liquid is washed with ethyl acetate 10ml, merges acetic acid
Ethyl ester liquid, recycling design, raffinate methanol are dissolved and are transferred in 10ml measuring bottle, are added methanol to scale, are shaken up, filter, take filter
Liquid to get.
Measuring method: accurate respectively to draw 5 μ l of reference extract solution, 10 μ l, test solution 5~l0 μ l infuses people's liquid phase
Chromatograph, measurement, is calculated separately in Bilobalide, ginkalide A, ginkolide B and ginkgo with external standard two-point method logarithmic equation
The content of ester C to get.
Measure supercritical extract ginkgo crude oil and ginkgo essential oil that molecular distillation is refined in total terpene lactone contents such as
Shown in table 4.
Table 4
| Total terpene lactone/% in supercritical extract ginkgo crude oil | Total terpene lactone/% in the ginkgo essential oil of purification | |
| Embodiment one | 0.0167 | 0.0211 |
| Embodiment two | 0.0189 | 0.0248 |
| Embodiment three | 0.0145 | 0.0207 |
Embodiment 7
The measurement of total carotinoid in ginkgo essential oil
Measuring method is referring to " changes of contents of Chinese azalea florescence petal carotenoid " and " carotenoids in yellow meat Peach fruits
Element extracts and study on determination method " (He Lisi, Xiao Zheng, Su Jiale, that waits Chinese azalea florescence petal carotenoid contains quantitative change
Change the Jiangsu forestry section, 44 (5): 18-21.；Yan Juan, Cai Zhixiang, Shen Zhijun, wait in Huang meat Peach fruits Extraction of carotenoid pigment and
Study on determination method Journal of Fruit Science, 2015,32 (6): 1267-1274.).
Carotenoid reference substance alpha-carotene, beta carotene and xanthophyll derive from Sigma company；Methanol and first
Base tertbutyl ether is chromatographically pure.
Agilent 1100 Infinity liquid chromatograph (1100 quaternary pump of Agilent, DAD detector, Agilent
1100 autosamplers, Agilent Chemstation software, Agilent Co., Ltd, the U.S.)；
Agilent Eclipse Plus C18 chromatographic column, (column length 150mm, column internal diameter 4.6mm, partial size are 5 μm).
The preparation of reference extract solution: alpha-carotene, beta carotene and each reference substance of xanthophyll are accurately weighed, first is used
The mixed standard solution that each standard items mass concentration is 20,10,1,0.2,0.1mg/L is prepared in alcohol dissolution.
The preparation of test solution: taking ginkgo raw sample/purification ginkgo essential oil about 2g, accurately weighed, sets tool plug taper
In bottle, precision plus people's methanol 10ml, weighed weight are protected from light, and ultrasonic 30min is let cool, and the weight of less loss is supplied with methanol, is shaken up,
Filtering, take filtrate to get.
Measuring method: with the mixed liquor (volume ratio 30: 70) of methyl tertiary butyl ether(MTBE) and methanol for mobile phase isocratic elution, stream
Speed be 1.0mL/min, Detection wavelength 450nm, 25 DEG C of column temperature, 20 μ L of sample volume.Infuse people's liquid chromatograph, measurement.Respectively will
Sample introduction is analyzed for the reference substance and test solution of each mass concentration, and peak area and reference substance content are carried out linear regression analysis,
Obtain standard curve regression equation.Corresponding α-Hu is calculated according to the peak area of test solution using standard curve regression equation
The content of radish element, beta carotene and xanthophyll ingredient, then to calculate carotenoid total amount as shown in table 5.
Table 5
Embodiment 8
The measurement of toxic component total ginkgoic acid in ginkgo essential oil
Specific measuring method is referring to " ginkgolic acid and total ginkgoic acid quantitative comparison in gingko different parts and different processed products "
(Chinese Pharmacopoeia Commission's Pharmacopoeia of People's Republic of China: one Beijing of version in 2015: China Medical Science Press, 2015:
416-417.；Lee turns plum, Zhang Xuelan, and Li Huifen waits ginkgolic acid and total ginkgoic acid in gingko different parts and different processed products fixed
Amount compares Chinese patent drug, 2015,37 (1): 164-168.).
Agilent 1100 Infinity liquid chromatograph (1100 quaternary pump of Agilent, DAD detector, Agilent
1100 autosamplers, Agilent Chemstation software, Agilent Co., Ltd, the U.S.)；
Agilent Eclipse Plus C18 chromatographic column, (column length 150mm, column internal diameter 4.6mm, partial size are 5 μm)；
Gingko eo-acid reference substance (Nat'l Pharmaceutical & Biological Products Control Institute),
Total ginkgoic acid reference substance (Nat'l Pharmaceutical & Biological Products Control Institute).
Using the acetonitrile containing 0.1% trifluoroacetic acid as mobile phase A, the water containing 0.1% trifluoroacetic acid is Mobile phase B, and gradient is washed
It is de-: 0-30min, 25-10%B；30-35min, 10%B.Detection wavelength is 310nm.
The preparation of test solution: taking ginkgo raw sample/purification ginkgo essential oil about 2g, accurately weighed, sets tool plug taper
In bottle, precision adds people's methanol 10ml, weighed weight, and ultrasonic 30min lets cool, the weight of less loss is supplied with methanol, is shaken up, and filters,
Take filtrate to get.
The preparation of reference substance solution: taking gingko eo-acid reference substance appropriate, accurately weighed, adds methanol that every lm L is made containing 100 μ
The solution of g, as reference substance solution；It separately takes total ginkgoic acid reference substance appropriate, the solution that every lm L contains 200 μ g is made with methanol,
As positioning contrast solution.
Measuring method: precision draws test solution, reference substance solution and each 50 μ L of positioning contrast solution, injects liquid phase color
Spectrometer, calculate test solution in chromatographic peak corresponding to total ginkgoic acid reference substance total peak area, with gingko eo-acid reference substance outside
Mark method calculate total ginkgoic acid content to get.
Measure supercritical extract ginkgo crude oil and ginkgo essential oil that molecular distillation is refined contained in total ginkgoic acid contain
Amount is as shown in table 6.
Table 6
Active constituent one of of the fatty acid as gingko, linoleic acid therein and conjugated linoleic acid lowering blood pressure and blood fat,
Prevention and cure of cardiovascular disease etc. plays a significant role.Intake is containing unsaturated fats such as oleic acid for the edible oil angle of health
Oil can delay aging, reduce the content of total cholesterol in blood.
Carotenoid has the multiple biological functions such as anti-oxidant, anticancer, is the nutriment beneficial to human body.Gingko
With the identical active constituent ginkgoterpene lactone of ginkgo leaf and flavones.The pharmacological action of gingko flavone compound and its antioxygen
Change, removing free radical has direct relationship, removes DPPH, superoxide anion, ABTS free radical and reducing power.Ginkgolides conduct
Generally acknowledged PAF receptor antagonist, the pharmacological action of antagonism PAF are sufficiently confirmed.Ginkgolides is
It is clinically used for the illnesss such as coronary heart disease, cerebral thrombosis, cerebral ischemia, brain disorder, brain injury sequelae, the nervous system disease and asthma
Treatment.Treatment of the existing sterling ginkgolides of foreign countries for apoplexy, organ transplant rejection, haemodialysis and shock etc.
Journey.
Ginkgo essential oil Sync enrichment that extracting method of the invention obtains unsaturated fatty acid, general flavone, Bilobalide,
Ginkgolide A. B. C, xanthophyll, β and alpha-carotene are more advantageous to human health relative to traditional vegetable oil.
The above specific embodiments are only exemplary, is to preferably make skilled artisans appreciate that originally
Patent, be not to be construed as include to this patent range limitation；As long as appointing made by the spirit according to disclosed in this patent
How with change or modification, the range that this patent includes is each fallen within.
Claims (10)
1. a kind of extracting method of ginkgo essential oil, which comprises the steps of:
S1 after ginkgo nut is mixed with water, carries out ultrasonic vibration and cyclonic separation processing, obtains food containing gingko almond particle；
S2, the food containing gingko almond particle that S1 is obtained carry out supercritical fluid extraction processing, obtain ginkgo nut crude oil；
S2 is obtained the progress molecular distillation of ginkgo nut crude oil and obtains ginkgo essential oil by S3.
2. the extracting method of ginkgo essential oil as described in claim 1, which is characterized in that mixed in ginkgo nut with water in the S1
Before, it further include that crush processing step is carried out to ginkgo nut.
3. the extracting method of ginkgo essential oil as described in claim 1, which is characterized in that in supercritical fluid extraction in the S2
Before processing, further includes: vacuum drying step.
4. the extracting method of ginkgo essential oil as described in claim 1, which is characterized in that in supercritical fluid extraction in the S2
Before processing, further includes: crush, screening step.
5. the extracting method of ginkgo essential oil as described in claim 1, which is characterized in that in supercritical fluid extraction in the S2
Before processing, further includes: air-flow broken wall pulverising step.
6. the extracting method of ginkgo essential oil as claimed in claim 5, which is characterized in that the air-flow broken wall pulverising step it
Afterwards, further includes: mixing and granulation step.
7. the extracting method of ginkgo essential oil as described in claim 1, which is characterized in that in supercritical fluid extraction in the S2
Before processing, further includes: microwave drying sterilization step.
8. the extracting method of ginkgo essential oil as described in claim 1, which is characterized in that in supercritical fluid extraction processing and divide
Between son distillation, further includes: solvent recovery and deodorization processing step.
9. the extracting method of ginkgo essential oil as described in claim 1, which is characterized in that in supercritical fluid extraction processing and divide
Between son distillation, further includes: refrigerated centrifuge step.
10. the extracting method of ginkgo essential oil as described in claim 1, which is characterized in that supercritical fluid extraction processing and
Between molecular distillation, further includes: vacuum filtration step.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110484372A (en) * | 2019-09-02 | 2019-11-22 | 徐州工业职业技术学院 | A kind of method of Semen Ginkgo extraction of essential oil |
| CN110551565A (en) * | 2019-10-09 | 2019-12-10 | 武汉轻工大学 | Processing production method of strong-fragrance pumpkin seed oil |
| CN114196479A (en) * | 2021-12-31 | 2022-03-18 | 广西膳君特医食品有限公司 | Low-temperature extraction process of ginkgo leaves |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050158398A1 (en) * | 2004-01-21 | 2005-07-21 | Ming Xie | Multifunctional nutrient supplement and a process for making |
| CN1737093A (en) * | 2005-08-11 | 2006-02-22 | 江苏同源堂生物工程有限公司 | Supercritical carbon dioxide extraction method for extracting gingko oil from gingko fruit |
| CN101935586A (en) * | 2010-09-28 | 2011-01-05 | 江苏江大源生态生物科技有限公司 | Method for extracting ganoderma spore oil with supercritical CO2 |
| CN104560403A (en) * | 2015-01-09 | 2015-04-29 | 成都宏亿实业集团有限公司 | Gingko essential oil and preparation method thereof |
| CN105638934A (en) * | 2016-02-23 | 2016-06-08 | 江苏佰康生物科技股份有限公司 | Gingko compound edible oil |
| CN105687035A (en) * | 2016-02-04 | 2016-06-22 | 江苏佰康生物科技股份有限公司 | Compound ginkgo essential oil with effects of resisting oxidation and delaying skin aging |
| CN107858207A (en) * | 2017-11-24 | 2018-03-30 | 广西中港高科国宝金花茶产业有限公司 | A kind of supercritical CO of golden flower tea essential oils2Extracting process |
-
2018
- 2018-07-25 CN CN201810826937.2A patent/CN109810789A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050158398A1 (en) * | 2004-01-21 | 2005-07-21 | Ming Xie | Multifunctional nutrient supplement and a process for making |
| CN1737093A (en) * | 2005-08-11 | 2006-02-22 | 江苏同源堂生物工程有限公司 | Supercritical carbon dioxide extraction method for extracting gingko oil from gingko fruit |
| CN101935586A (en) * | 2010-09-28 | 2011-01-05 | 江苏江大源生态生物科技有限公司 | Method for extracting ganoderma spore oil with supercritical CO2 |
| CN104560403A (en) * | 2015-01-09 | 2015-04-29 | 成都宏亿实业集团有限公司 | Gingko essential oil and preparation method thereof |
| CN105687035A (en) * | 2016-02-04 | 2016-06-22 | 江苏佰康生物科技股份有限公司 | Compound ginkgo essential oil with effects of resisting oxidation and delaying skin aging |
| CN105638934A (en) * | 2016-02-23 | 2016-06-08 | 江苏佰康生物科技股份有限公司 | Gingko compound edible oil |
| CN107858207A (en) * | 2017-11-24 | 2018-03-30 | 广西中港高科国宝金花茶产业有限公司 | A kind of supercritical CO of golden flower tea essential oils2Extracting process |
Non-Patent Citations (1)
| Title |
|---|
| 袁惠新: "《分离工程》", 31 January 2002, 中国石化出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110484372A (en) * | 2019-09-02 | 2019-11-22 | 徐州工业职业技术学院 | A kind of method of Semen Ginkgo extraction of essential oil |
| CN110551565A (en) * | 2019-10-09 | 2019-12-10 | 武汉轻工大学 | Processing production method of strong-fragrance pumpkin seed oil |
| CN114196479A (en) * | 2021-12-31 | 2022-03-18 | 广西膳君特医食品有限公司 | Low-temperature extraction process of ginkgo leaves |
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