CN108553498A - A kind of saussurea involucrata essence extraction process - Google Patents
A kind of saussurea involucrata essence extraction process Download PDFInfo
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- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
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- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
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Abstract
The present invention discloses a kind of saussurea involucrata essence extraction process, is removed the peel by soaking and washing, and by saussurea involucrata using going the pure water of deionization to impregnate, immersion is finished carries out cleaning peeling to saussurea involucrata;Saussurea involucrata after being removed the peel to soaking and washing carries out cutting, saussurea involucrata particle after cutting is ground, grinding is ground alternately with counterclockwise clockwise when grinding, ultrasonic disruption is carried out to the saussurea involucrata after grinding, by ultrasonic disruption, treated that saussurea involucrata extracts, extraction, which finishes, to be filtered, and extraction filtrate is obtained;Extraction filtrate is centrifuged to obtain centrifugation supernatant liquor, supernatant liquor is taken to be extracted;Solvent recovery is carried out to the supernatant liquor of second of centrifugation, and cleaned, purified;Saussurea involucrata extracting solution after clarification is concentrated and dried, saussurea involucrata essence finished product, 70% or more saussurea involucrata essence extraction rate reached are obtained, the present invention can fully extract the essence of saussurea involucrata, retain the active ingredient in saussurea involucrata to greatest extent, meets industrialization production requirements, benefit is brought to enterprise.
Description
Technical field
The present invention relates to a kind of saussurea involucrata essence extraction processes, belong to technical field of plant extraction.
Background technology
Saussurea involucrata, also known as sub- tribute, chrysanthemum potato, join fruit etc..For the dicotyledonous herbaceous plant for many years of composite family Helianthus.Yacon
The actually root tuber of under ground portion, shape is like sweet potato, raw ripe all edibles.Saussurea involucrata was needed from germinateing to blooming after 5 years, kind
Son germinates in zero degrees celsius, and three to five degrees Celsius of growths, seedling can resist subzero 21 degrees Celsius of low temperature, actual
Growth period, in this short growth period, saussurea involucrata can exceed that by feat of vigorous vitality, plant height but less than two months
Five to seven times of other plants.Fruit is root tuber, and pericarp is canescence, and pulp is faint yellow, and shape is tasted as sweet potato, pulp, mouth
Sense is but like pyrus nivalis, and glittering and translucent and succulence is fragrant and sweet crisp and refreshing, is a kind of pure natural medicinal fruit.Yacon is low-heat food
Product, the DF in pulp have important physiological function, can promote enterogastric peristalsis, relax bowel, eliminate constipation, slim beauty treatment, drop
Hypoglycemia, prevention and treatment hypertension, obesity, diabetes and cardiovascular and cerebrovascular disease and other effects.Yacon contains abundant
Fructooligosaccharide, fructooligosaccharide are primarily present in yacon stem tuber, and content is the 45%-65% of dry matter, the fructooligosaccharide in yacon
It is that content is highest in all plants, is that Bifidobacterium Bifidum breeds required nutritional ingredient in human body, yacon is special because of its
Functional characteristic and good medical value and its part that do not developed are increasingly paid attention to.
The Chinese patent of Publication No. CN104274348A discloses a kind of preparation method of saussurea involucrata essence, including raw material
Processing step, solvent extraction step, extraction step, purification step, preparation steps, finally obtain form be solution, paste or
The saussurea involucrata essence finished product of one of pulvis, the invention crush saussurea involucrata herb, then with solvent extraction, obtain extracting solution, then removal of impurities,
Purifying, then is prepared with solvent, obtains the saussurea involucrata essence for being not added with preservative, the saussurea involucrata essence produced, polyoses content and total
Flavones content is stablized, and " total plate count ", " yeast and mold " and " escherichia coli " number in control range, meets and sets
Meter requires, and can be added in daily chemical products and use directly as additive or active constituent, the preparation method is in industrialized production
Middle practice obtains the saussurea involucrata essence consistent with laboratory scale product, meets industrialization production requirements.
The Chinese patent of Publication No. CN103550275A discloses a kind of extracting method of saussurea involucrata essence substance, including
Following steps:(1) pretreatment of saussurea involucrata and purified water;(2) obtained saussurea involucrata will be pre-processed and pure water extracts;It (3) will be cold
But accurate separation is carried out after the saussurea involucrata soup coarse filtration after;(4) with aperture it is again 0.25-0.45um microporous barriers by secondary filter liquid
Filtering;(5) polishing purification liquid is concentrated at normal temperatures with reverse osmosis membrane;(6) by the saussurea involucrata soup by reverse osmosis membrane concentration
It is concentrated under reduced pressure again;(7) essence extract is finally obtained.
The extracting method of the prior art, it is relatively high to performance, the control accuracy requirement of production procedure of process equipment,
And the pipeline arrangement of related upstream and downstream equipment is intricate, the production cost is very high.The method of Mechanical Crushing cell cannot be by cell
It is crushed to required degree, the method for chemically fragmenting is easy to cause the active change of institute's extract again, and can also be along with extraction
Pollution problem, cost is also higher, thus is difficult to obtain ideal effect.Ultrasonic technology be widely used at present electronics,
The industries such as machinery and light industry.Ultrasonic extraction is that Ultrasonic Radiation pressure is utilized, and increases molecular motion of material frequency and speed
Degree increases solvent penetration power and promotes the progress of extraction to accelerate target component to enter solvent.
Invention content
The present invention is in view of the deficienciess of the prior art, provide a kind of saussurea involucrata essence extraction process, based on ultrasonic wave skill
Art can fully extract the essence of saussurea involucrata, greatly promote nutrition absorption rate, remain to the maximum extent effective in saussurea involucrata
Ingredient, extraction effect is good, efficient, cost-effective, environment friendly and pollution-free.
The technical solution that the present invention solves above-mentioned technical problem is as follows:A kind of saussurea involucrata essence extraction process, feature exist
In:The extraction process includes the following steps:
(1) soaking and washing is removed the peel, and by saussurea involucrata using going the pure water of deionization to impregnate, soaking time is 3 to 6 hours,
Soaking temperature is 4 to 10 DEG C, and immersion is finished carries out cleaning peeling to saussurea involucrata;
(2) cutting, the saussurea involucrata after being removed the peel to soaking and washing carry out cutting, are cut into that grain size length and width are 3 to 10mm
Grain;
(3) slurrying is ground, the saussurea involucrata particle after cutting is ground, grinding and counterclockwise grinding clockwise when grinding
Alternately, each milling time is 1 to 2min, and the control of total milling time is 4 to 8min;
(4) ultrasonic disruption carries out ultrasonic disruption to the saussurea involucrata after grinding, and ultrasonic power is 160 to 300W, is surpassed
Sonication times are 1 to 9min, and it is 35 to 60 DEG C to be ultrasonically treated temperature;
(5) extraction filtering, by ultrasonic disruption, treated that saussurea involucrata extracts, and extraction time is 10 to 20min, leaching
It carries finishing and be filtered, obtain extraction filtrate;
(6) it centrifuges for the first time, carrying out centrifugation for the first time in 3000r/min to extraction filtrate obtains centrifugation supernatant liquor, takes
Supernatant liquor is extracted;
(7) it centrifuges for second, phase on the extract liquor after extraction is taken to be centrifuged for second in 5000r/min progress
Supernatant liquor;
(8) clarification carries out solvent recovery to the supernatant liquor of second of centrifugation, and is cleaned, purified;
(9) it is concentrated and dried, the saussurea involucrata extracting solution after clarification is concentrated and dried, saussurea involucrata essence finished product is obtained.
A kind of saussurea involucrata essence extraction process as described above in the step (3), is ground in pulping process, in mortar plus
Enter the phosphate buffer containing EDTA, mortar is rinsed 2 to 3 times with the phosphate buffer containing EDTA again, obtains milled mixtures.
EDTA (ethylenediamine tetra-acetic acid) is a kind of excellent calcium and magnesium ion chelating agent, is used as the chelating agent of water used in emulsion polymerization, removes
Remove Ca2+、Mg2+、Fe2+、Fe3+Equal metal ions.
A kind of saussurea involucrata essence extraction process as described above, in the step (4), cellulose is added in when ultrasonic disruption
Enzyme is hydrolyzed, and the cellulase uses the fiber of model Validase TRL and the Rapidase TF of Royal DSM company
The mass ratio of the mixture of plain enzyme, two kinds of cellulases is 4:5, the quality of the mixture of the cellulase is the saussurea involucrata
The 0.03% of lapping liquid quality, in the step (5), extraction filtrate temperature control is 75 to 85 DEG C, to the fibre in extraction filtrate
The plain enzyme of dimension is inactivated.
A kind of saussurea involucrata essence extraction process as described above, in the step (6), for the first time the time of centrifugation be 10 to
20min is extracted using 3: 5 chloroform-ethyl alcohol, and the ratio of extractant and extract liquor is 1: 2.5.
A kind of saussurea involucrata essence extraction process as described above, in the step (7), time of second of centrifugation be 10 to
20min。
A kind of saussurea involucrata essence extraction process as described above in the step (8), passes through macroporous resin adsorption, alcohol
It is heavy, water is heavy, one or a combination set of membrane filtering method carries out clarification.
A kind of saussurea involucrata essence extraction process as described above, it is dry using microwave vacuum low-temperature, true in the step (9)
Vacuum freecing-dry or one or a combination set of the method for spray drying are concentrated and dried.
A kind of saussurea involucrata essence extraction process as described above,:The saussurea involucrata is snow lotus of big bud, Saussurea medusa or bract snow
One kind in lotus.
A kind of saussurea involucrata essence extraction process as described above, the saussurea involucrata essence finished product be solution, paste or pulvis it
One.
The beneficial effects of the invention are as follows:The present invention is removed the peel by soaking and washing, by saussurea involucrata using go the pure water of deionization into
Row impregnates, and immersion is finished carries out cleaning peeling to saussurea involucrata;Saussurea involucrata after being removed the peel to soaking and washing carries out cutting, after cutting
Saussurea involucrata particle is ground, when grinding clockwise grinding and counterclockwise grinding alternately, ultrasound is carried out to the saussurea involucrata after grinding
Wave is broken, and by ultrasonic disruption, treated that saussurea involucrata extracts, and extraction, which finishes, to be filtered, and extraction filtrate is obtained;To extraction
Filtrate is centrifuged to obtain centrifugation supernatant liquor, and supernatant liquor is taken to be extracted;The supernatant liquor of second of centrifugation is carried out molten
Agent is recycled, and is cleaned, purified;Saussurea involucrata extracting solution after clarification is concentrated and dried, obtain saussurea involucrata essence at
Product.The present invention is based on ultrasonic technologies, can fully extract the essence of saussurea involucrata, greatly promote nutrition absorption rate, to the maximum extent
The active ingredient in saussurea involucrata is remained, extraction effect is good, efficient, cost-effective, environment friendly and pollution-free, meets industrial metaplasia
Production requires, and benefit is brought to enterprise.
Specific implementation mode
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, it elaborates in the following description
Many details are in order to fully understanding the present invention.But the present invention can be to be much different from other sides described here
Formula is implemented, and those skilled in the art can make similar improvements without departing from the spirit of the invention, therefore the present invention is not
It is limited by following public specific embodiment.
Embodiment one
40 grams of yacons are taken, by yacon using going the pure water of deionization to impregnate, soaking time is 3 hours, is impregnated
Temperature is 4 DEG C, and immersion is finished carries out cleaning peeling to saussurea involucrata;Saussurea involucrata after being removed the peel to soaking and washing carries out cutting, cutting granulating
Diameter length and width are the particle of 3mm;Saussurea involucrata particle after cutting is ground, when grinding clockwise grinding and counterclockwise grinding hand over
For progress, each milling time is 1min, and the control of total milling time is 4min;It is broken that ultrasonic wave is carried out to the saussurea involucrata after grinding
Broken, ultrasonic power 160W, ultrasonic treatment time 1min, it is 35 DEG C to be ultrasonically treated temperature;Ultrasonic disruption is handled
Saussurea involucrata afterwards is extracted, extraction time 10min, and extraction, which finishes, to be filtered, and obtains extraction filtrate;Exist to extraction filtrate
3000r/min carries out centrifugation for the first time and obtains centrifugation supernatant liquor, and supernatant liquor is taken to be extracted;Take the extract liquor after extraction
Upper phase carries out second of centrifugation in 5000r/min and obtains centrifugation supernatant liquor;Solvent is carried out to the supernatant liquor of second of centrifugation
Recycling, and cleaned, purified;Saussurea involucrata extracting solution after clarification is concentrated and dried, saussurea involucrata essence finished powder is obtained
28.5 grams of agent, essence recovery rate about 71%.
Embodiment two
40 grams of yacons are taken, by yacon using going the pure water of deionization to impregnate, soaking time is 4 hours, is impregnated
Temperature is 6 DEG C, and immersion is finished carries out cleaning peeling to saussurea involucrata;Saussurea involucrata after being removed the peel to soaking and washing carries out cutting, cutting granulating
Diameter length and width are the particle of 7mm;Saussurea involucrata particle after cutting is ground, when grinding clockwise grinding and counterclockwise grinding hand over
For progress, each milling time is 1.5min, and the control of total milling time is 6min;Ultrasonic wave is carried out to the saussurea involucrata after grinding
Broken, ultrasonic power 250W, ultrasonic treatment time 5min, it is 50 DEG C to be ultrasonically treated temperature;At ultrasonic disruption
Saussurea involucrata after reason is extracted, extraction time 15min, and extraction, which finishes, to be filtered, and obtains extraction filtrate;To extracting filtrate
Centrifugation for the first time is carried out in 3000r/min and obtains centrifugation supernatant liquor, and supernatant liquor is taken to be extracted;Take the extraction after extraction
Mutually second of centrifugation is carried out in 5000r/min obtain centrifugation supernatant liquor on liquid;The supernatant liquor of second of centrifugation is carried out molten
Agent is recycled, and is cleaned, purified;Saussurea involucrata extracting solution after clarification is concentrated and dried, saussurea involucrata essence finished product is obtained
31.8 grams of pulvis, essence recovery rate about 79.5%.
Embodiment three
40 grams of yacons are taken, by yacon using going the pure water of deionization to impregnate, soaking time is 6 hours, is impregnated
Temperature is 10 DEG C, and immersion is finished carries out cleaning peeling to saussurea involucrata;Saussurea involucrata after being removed the peel to soaking and washing carries out cutting, is cut into
Grain size length and width are the particle of 10mm;Saussurea involucrata particle after cutting is ground, grinding and counterclockwise grinding clockwise when grinding
Alternately, each milling time is 2min, and the control of total milling time is 8min;Ultrasonic wave is carried out to the saussurea involucrata after grinding
Broken, ultrasonic power 300W, ultrasonic treatment time 9min, it is 60 DEG C to be ultrasonically treated temperature;At ultrasonic disruption
Saussurea involucrata after reason is extracted, extraction time 20min, and extraction, which finishes, to be filtered, and obtains extraction filtrate;To extracting filtrate
Centrifugation for the first time is carried out in 3000r/min and obtains centrifugation supernatant liquor, and supernatant liquor is taken to be extracted;Take the extraction after extraction
Mutually second of centrifugation is carried out in 5000r/min obtain centrifugation supernatant liquor on liquid;The supernatant liquor of second of centrifugation is carried out molten
Agent is recycled, and is cleaned, purified;Saussurea involucrata extracting solution after clarification is concentrated and dried, saussurea involucrata essence finished product is obtained
30.2 grams of pulvis, essence recovery rate about 75.5%.
The present invention is removed the peel by soaking and washing, and by saussurea involucrata using going the pure water of deionization to impregnate, immersion is finished to snow
Lotus carries out cleaning peeling;Saussurea involucrata after being removed the peel to soaking and washing carries out cutting, is ground, grinds to the saussurea involucrata particle after cutting
Grinding and grinding counterclockwise alternately, carry out ultrasonic disruption, by ultrasonic disruption to the saussurea involucrata after grinding clockwise when mill
Treated, and saussurea involucrata is extracted, and extraction, which finishes, to be filtered, and obtains extraction filtrate;To extraction filtrate centrifuged to obtain from
Heart supernatant liquor, takes supernatant liquor to be extracted;Solvent recovery is carried out to the supernatant liquor of second of centrifugation, and cleaned,
Purifying;Saussurea involucrata extracting solution after clarification is concentrated and dried, saussurea involucrata essence finished product is obtained, whole saussurea involucrata essence carries
It takes rate to reach 70% or more, can fully extract the essence of saussurea involucrata, greatly promote nutrition absorption rate, remain to the maximum extent
Active ingredient in saussurea involucrata, extraction effect is good, efficient, cost-effective, environment friendly and pollution-free, meets industrialization production requirements,
Benefit is brought to enterprise.
Each technical characteristic of embodiment described above can be combined arbitrarily, to keep description succinct, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, it is all considered to be the range of this specification record.
Several embodiments of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (9)
1. a kind of saussurea involucrata essence extraction process, it is characterised in that:The extraction process includes the following steps:
(1) soaking and washing is removed the peel, and by saussurea involucrata using going the pure water of deionization to impregnate, soaking time is 3 to 6 hours, is impregnated
Temperature is 4 to 10 DEG C, and immersion is finished carries out cleaning peeling to saussurea involucrata;
(2) cutting, the saussurea involucrata after being removed the peel to soaking and washing carry out cutting, are cut into the particle that grain size length and width are 3 to 10mm;
(3) grind slurrying, the saussurea involucrata particle after cutting be ground, when grinding clockwise grinding and counterclockwise grinding alternately into
Row, each milling time are 1 to 2min, and the control of total milling time is 4 to 8min;
(4) ultrasonic disruption carries out ultrasonic disruption to the saussurea involucrata after grinding, and ultrasonic power is 160 to 300W, at ultrasonic wave
It is 1 to 9min to manage the time, and it is 35 to 60 DEG C to be ultrasonically treated temperature;
(5) extraction filtering, by ultrasonic disruption, treated that saussurea involucrata extracts, and extraction time is 10 to 20min, and extraction finishes
It is filtered, obtains extraction filtrate;
(6) it centrifuges for the first time, carrying out centrifugation for the first time in 3000r/min to extraction filtrate obtains centrifugation supernatant liquor, takes upper layer
Clear liquid is extracted;
(7) it second centrifuges, takes on the extract liquor after extraction and mutually to carry out second of centrifugation in 5000r/min to obtain centrifugation upper layer clear
Liquid;
(8) clarification carries out solvent recovery to the supernatant liquor of second of centrifugation, and is cleaned, purified;
(9) it is concentrated and dried, the saussurea involucrata extracting solution after clarification is concentrated and dried, saussurea involucrata essence finished product is obtained.
2. a kind of saussurea involucrata essence extraction process according to claim 1, it is characterised in that:In the step (3), grinding system
During slurry, the phosphate buffer containing EDTA is added in mortar, mortar is rinsed 2 to 3 times with the phosphate buffer containing EDTA, obtained again
Obtain milled mixtures.
3. a kind of saussurea involucrata essence extraction process according to claim 1, it is characterised in that:In the step (4), ultrasonic wave
Cellulase is added when broken to be hydrolyzed, the cellulase using Royal DSM company model Validase TRL and
The mass ratio of the mixture of the cellulase of Rapidase TF, two kinds of cellulases is 4:5, the mixture of the cellulase
Quality be the 0.03% of the saussurea involucrata lapping liquid quality, in the step (5), extraction filtrate temperature control is 75 to 85 DEG C,
Cellulase in extraction filtrate is inactivated.
4. a kind of saussurea involucrata essence extraction process according to claim 1, it is characterised in that:In the step (6), for the first time
The time of centrifugation is 10 to 20min, is extracted using 3: 5 chloroform-ethyl alcohol, and the ratio of extractant and extract liquor is 1:
2.5。
5. a kind of saussurea involucrata essence extraction process according to claim 1, it is characterised in that:In the step (7), second
The time of centrifugation is 10 to 20min.
6. a kind of saussurea involucrata essence extraction process according to claim 1, it is characterised in that:In the step (8), lead to
Cross that macroporous resin adsorption, alcohol precipitation, water is heavy, one or a combination set of membrane filtering method carries out clarification.
7. a kind of saussurea involucrata essence extraction process according to claim 1, it is characterised in that:In the step (9), use is micro-
One or a combination set of wave vacuum dehydrating at lower temperature, vacuum freeze drying or method of spray drying are concentrated and dried.
8. a kind of saussurea involucrata essence extraction process according to claim 1, it is characterised in that:The saussurea involucrata is snow lotus of big bud,
One kind in Saussurea medusa or Saus-surea obvallata (DC.) Edgew.
9. a kind of saussurea involucrata essence extraction process according to claim 1, it is characterised in that:The saussurea involucrata essence finished product is molten
One of liquor, paste or pulvis.
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Cited By (2)
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CN113717250A (en) * | 2021-11-02 | 2021-11-30 | 烟台金蕊女性用品有限公司 | Saussurea involucrate micromolecule polypeptide, extraction process and application thereof |
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CN113717250B (en) * | 2021-11-02 | 2022-02-18 | 烟台金蕊女性用品有限公司 | Saussurea involucrate micromolecule polypeptide, extraction process and application thereof |
CN116695273A (en) * | 2023-05-17 | 2023-09-05 | 百事基材料(青岛)股份有限公司 | Nylon large biological fiber containing saussurea involucrata active ingredient and preparation method thereof |
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