CN107602641A - A kind of method based on freeze-drying ultra high pressure extraction otoginsenoside from buckeye - Google Patents
A kind of method based on freeze-drying ultra high pressure extraction otoginsenoside from buckeye Download PDFInfo
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- CN107602641A CN107602641A CN201710665124.5A CN201710665124A CN107602641A CN 107602641 A CN107602641 A CN 107602641A CN 201710665124 A CN201710665124 A CN 201710665124A CN 107602641 A CN107602641 A CN 107602641A
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Abstract
The invention discloses a kind of method based on freeze-drying ultra high pressure extraction otoginsenoside from buckeye, it is first to be freeze-dried buckeye medicinal material after crushing, soaking, then ultra high pressure extraction is carried out again, and extraction step includes boost phase, packing stage, pressure release stage etc..The present invention by buckeye by carrying out freeze-drying process, so as to change the internal structure of medicinal material tissue, makes cell membrane be easier to rupture, and active component is easier to ooze out, and so as to reduce the pressure of ultra high pressure extraction and number, reduces energy consumption and cost.
Description
Technical field
The invention belongs to pharmaceutical field, is related to the extracting method of otoginsenoside, especially a kind of to be based on freeze-drying from Suo
The method of ultra high pressure extraction otoginsenoside in Luo Zi.
Background technology
Otoginsenoside is also known as otoginsenoside acid, be extract to obtain from Hippocastanaceae buckeye seed total saposins,
The general name of β-otoginsenoside or different otoginsenoside etc., belongs to triterpene saponin.Otoginsenoside has a variety of work(such as anti-inflammatory, antioedematous
Effect, clinically it is mainly used in the treatment of the diseases such as encephaledema, wound.At present the extraction overwhelming majority to otoginsenoside using
The method of alcohol heat reflux or seepage, such as CN 104402963 A, CN 102659897 A, CN 106589045 A, CN
The patent documents such as 104804060 A are using such method.
With the continuous progress of traditional Chinese medicine extraction technology, increasing new method is used for carrying for otoginsenoside active component
In taking.The A of CN 106491672 disclose a kind of method of the supercritical carbon dioxide extracting extraction otoginsenoside of use, CN
106554384 A disclose the method using ultrasound assisted extraction otoginsenoside, and the A of CN 102309529 are disclosed using microwave
The method for extracting otoginsenoside, the A of CN 101967175 disclose the method using Ultrasonic-microwave synergistic extraction otoginsenoside.
But the report of super-pressure method extraction otoginsenoside is used until having not yet to see.
Ultra high pressure extraction is also referred to as the extraction of superelevation isostatic cool pressing, refers to 100-1000MPa hydrostatic pressure in carrying
On the mixed liquor for taking solvent and Chinese medicine, and a period of time is kept under a predetermined, plant cell external and internal pressure is reached balance
Rapid release afterwards.Because intraor extracellular osmotic pressure increases suddenly, the structure of cell membrane changes so that intracellular is effective
Composition can pass through cell membrane and be transferred in extracellular extract solution, reach the purpose of extraction effective component of chinese medicine.This method
A variety of effective ingredients such as flavones in medicinal material, saponin(e, polysaccharide and alkaloid can effectively be extracted.Compared with other extracting modes, surpass
High pressure extraction has the advantages that temperature is low, the time is short, efficiency high.
Buckeye quality is hard, and cell membrane is difficult to rupture, and solvent is difficult to infiltrate through medicinal material tissue, when causing ultra high pressure extraction
Higher pressure (it is generally necessary to more than 500Mpa) and more number (it is generally necessary to repeating extraction more than 3 times) are needed, so as to increase
Energy consumption and cost are added.
The content of the invention
It is an object of the invention to provide a kind of method of ultra high pressure extraction otoginsenoside, this method is first carried out buckeye
Freeze-drying process, so as to change the internal structure of medicinal material tissue, cell membrane is set to be easier to rupture, active component is easier to ooze
Go out, so as to reduce the pressure of ultra high pressure extraction and number, reduce energy consumption and cost.
Method provided by the invention comprises the following steps：
(1) buckeye is crushed into the powder for 5-100 mesh granularities, is pulled out after soaking 0.5-3 hours, drain surface
Moisture, it is placed in household freezer and freezes rapidly；
(2) buckeye after freezing is dried in vacuo, controls the vacuum of drying process in the range of 10-20pa,
Temperature is in the range of 10-50 DEG C；
(3) Extraction solvent of 5-20 times of weight is added into dried buckeye, loads pressure-resistant, flexible soft bag together
Middle sealing, it is then placed in the extraction vessel of ultra high pressure extraction device, is extracted at normal temperatures, extraction step is as follows：
1) boost phase：The pressure in extraction vessel is increased to 100-400Mpa in 5-30min；
2) packing stage：Keep pressure 5-20min；
3) the pressure release stage：Pressure is let out as normal pressure rapidly in 5-30s；
4) repeat step 1) -3) 1-3 times；
(4) soft bag is taken out from ultra high pressure extraction device, pours out material, it is filtered, centrifuge, concentration, produced after drying
Otoginsenoside extract.
Preferably, the Extraction solvent is water or 10-50% ethanol.According to the similar principle that mixes, using the solvent extraction
Active component content highest.
Preferably, the granularity of the Buckeye Seed is 10-30 mesh.Particle diameter is excessive, and solvent cannot easily penetrate medicinal material infiltration
To histocyte, contact of the active component with solvent is reduced, and causes extraction efficiency to reduce；, whereas if particle diameter is too small, then not only
The dissolution of the impurity constituents such as active component dissolution increase, medicinal material tissue, albumen, tannin can also increase, and can cause to extract on the contrary
Active component content in thing reduces.
Preferably, the Extraction solvent is 10-15 times of buckeye weight.Very little, then active component reaches Extraction solvent
It is difficult to continue dissolution after dissolution equilibrium, causes extraction efficiency not high, solvent can then increase cost too much.
Preferably, the boost phase is that the pressure in extraction vessel is increased into 200-300Mpa in 10-15min.
Pressure is higher, then the transmission speed of solvent infiltration and active component is faster, while can also influence solvent density, activity and medicinal material base
Block structure, accelerate the dissolution rate of active component, stripping quantity increase；But if hypertonia, can equally make impuritiess into
Point dissolution increase, to extracting unfavorable on the contrary and can increase cost.And the faster cell membrane of speed to boost is more easily broken.
Preferably, the time of the packing stage is 10-15min.Within this range, the dissolving of solute can preferably reach
Balance.
Preferably, the time in the pressure release stage is 10-15s.The histiocytic pressure of medicinal material is from hundreds of MPas of superelevation
Pressure is kept to normal pressure rapidly, in the presence of buffer brake, the explosion expansion of fluid and medicinal material matrix volume occurs, to medicinal material group
Knit and to form strong impact and cause to deform upon, while loose, hole, rupture occurs in eucaryotic cell structure, makes medicinal ingredient and solvent
Fully contact and outwards rapid diffusion.Therefore, venting duration should be more short better in theory, but if the time is too short, then can lead
Cause a large amount of invalid components dissolutions.
Preferably, repeat step 1) -3) 1 time, the active component of extraction is not only abundant, and shortens the cycle and save the energy.
Involved concentration of alcohol refers both to volumetric concentration in the present invention, as 10-50% ethanol refers to every 100ml ethanol
Contain ethanol 10-50ml in the aqueous solution.
The beneficial effects of the invention are as follows：
1) using the method for the present invention, compared with existing extracting method, it is possible to increase otoginsenoside contains in extract
Amount, impurity being reduced, while the rate of transform of otoginsenoside can also be improved, illustrate that medicinal material utilization rate is higher, extraction is more abundant, so as to
Reduce extraction cost.
2) compared with the extracting methods such as hot backflow, decoction, microwave, ultrasound, the present invention enters at relatively low temperature (room temperature)
OK, destroyed so as to reduce energy resource consumption and active component, obtained extract has more preferable medical active.
3) pre-treatment of the invention and extraction time are no more than 5 hours altogether, and wherein the time of ultra high pressure extraction is not altogether
More than 3 hours, compared with the conventional method, extraction time is greatly shortened, improves extraction efficiency.
4) pretreatment of the invention before ultra high pressure extraction, being freeze-dried to buckeye medicinal material, medicinal material first pass through
Immersion, substantial amounts of moisture content penetrate into medicinal material organization internal, the principle of ice crystal distillation are then recycled, in the environment of high vacuum
Under, without melting directly from ice solid sublimation be steam by frozen moisture, moisture during distillation spilling,
Medicinal material organization internal leaves a large amount of holes, medicinal material organization internal is formed porous spongelike structure so that super-pressure it is molten
Agent can be easier to penetrate into histocyte through medicinal material and extract active component, so as to advantageously reduce the pressure of super-pressure
Extraction time that is strong and reducing super-pressure, and then reduce energy consumption and cost.
Concrete facts mode
The present invention is described in detail below by specific embodiment.
Embodiment 1
(1) buckeye is crushed into the powder for 15 mesh granularities, is pulled out after soaking 2 hours, drain the moisture on surface, put
Freezed rapidly in the household freezer that temperature is -25 DEG C；
(2) buckeye after freezing is dried in vacuo, the vacuum for controlling drying process is 10pa, temperature 40
℃；
(3) 20% ethanol of 12 times of weight is added into dried buckeye, is fitted into together in pressure-resistant, flexible soft bag
Sealing, is then placed in the extraction vessel of ultra high pressure extraction device, is extracted at normal temperatures, extraction step is as follows：
1) boost phase：The pressure in extraction vessel is increased to 200Mpa in 15min；
2) packing stage：Keep pressure 15min；
3) the pressure release stage：Pressure is let out as normal pressure rapidly in 10s；
4) repeat step 1) -3) 1 time；
(4) soft bag is taken out from extraction vessel, pours out material, it is filtered, centrifuge, concentration, seven leaf soaps are produced after drying
Glucoside extract.
Through measuring and calculating, extract yield 16.3%, otoginsenoside purity is 49.6%, the otoginsenoside rate of transform 99.6%.
Embodiment 2
(1) buckeye is crushed into the powder for 30 mesh granularities, is pulled out after soaking 3 hours, drain the moisture on surface, put
Freezed rapidly in the household freezer that temperature is -30 DEG C；
(2) buckeye after freezing is dried in vacuo, the vacuum for controlling drying process is 20pa, temperature 50
℃；
(3) water of 15 times of weight is added into dried buckeye, is fitted into together in pressure-resistant, flexible soft bag and seals,
It is then placed in ultra high pressure extraction device, is extracted at normal temperatures, extraction step is as follows：
1) boost phase：The pressure in extraction vessel is increased to 300Mpa in 10min；
2) packing stage：Keep pressure 10min；
3) the pressure release stage：Pressure is let out as normal pressure rapidly in 15s；
4) repeat step 1) -3) 2 times；
(4) soft bag is taken out from ultra high pressure extraction device, pours out material, it is filtered, centrifuge, concentration, produced after drying
Otoginsenoside extract.
Through measuring and calculating, extract yield 17.1%, otoginsenoside purity is 47.0%, the otoginsenoside rate of transform 99.0%.
Embodiment 3
(1) buckeye is crushed into the powder for 10 mesh granularities, is pulled out after soaking 1 hour, drain the moisture on surface, put
Freezed rapidly in the household freezer that temperature is -20 DEG C；
(2) buckeye after freezing is dried in vacuo, the vacuum for controlling drying process is 15pa, temperature 30
℃；
(3) 30% ethanol of 10 times of weight is added into dried buckeye, is fitted into together in pressure-resistant, flexible soft bag
Sealing, is then placed in the extraction vessel of ultra high pressure extraction device, is extracted at normal temperatures, extraction step is as follows：
1) boost phase：The pressure in extraction vessel is increased to 250Mpa in 15min；
2) packing stage：Keep pressure 20min；
3) the pressure release stage：Pressure is let out as normal pressure rapidly in 5s；
4) repeat step 1) -3) 3 times；
(4) soft bag is taken out from ultra high pressure extraction device, pours out material, it is filtered, centrifuge, concentration, produced after drying
Otoginsenoside extract.
Through measuring and calculating, extract yield 17.3%, otoginsenoside purity is 46.3%, the otoginsenoside rate of transform 98.7%.
Embodiment 4
(1) buckeye is crushed into the powder for 5 mesh granularities, is pulled out after soaking 3 hours, drain the moisture on surface, put
Freezed rapidly in the household freezer that temperature is -30 DEG C；
(2) buckeye after freezing is dried in vacuo, the vacuum for controlling drying process is 10pa, temperature 25
℃；
(3) 50% ethanol of 20 times of weight is added into dried buckeye, is fitted into together in pressure-resistant, flexible soft bag
Sealing, is then placed in the extraction vessel of ultra high pressure extraction device, is extracted at normal temperatures, extraction step is as follows：
1) boost phase：The pressure in extraction vessel is increased to 400Mpa in 20min；
2) packing stage：Keep pressure 10min；
3) the pressure release stage：Pressure is let out as normal pressure rapidly in 30s；
4) repeat step 1) -3) 2 times；
(4) soft bag is taken out from ultra high pressure extraction device, pours out material, it is filtered, centrifuge, concentration, produced after drying
Otoginsenoside extract.
Through measuring and calculating, extract yield 16.8%, otoginsenoside purity is 47.2%, the otoginsenoside rate of transform 97.6%.
Embodiment 5
(1) buckeye is crushed into the powder for 50 mesh granularities, is pulled out after soaking 1 hour, drain the moisture on surface, put
Freezed rapidly in household freezer；
(2) buckeye after freezing is dried in vacuo, controls the vacuum of drying process in the range of 10~20pa,
Temperature is in the range of 10-50 DEG C；
(3) 40% ethanol of 5 times of weight is added into dried buckeye, is fitted into together in pressure-resistant, flexible soft bag
Sealing, is then placed in the extraction vessel of ultra high pressure extraction device, is extracted at normal temperatures, extraction step is as follows：
1) boost phase：The pressure in extraction vessel is increased to 100Mpa in 5-30min；
2) packing stage：Keep pressure 20min；
3) the pressure release stage：Pressure is let out as normal pressure rapidly in 5s；
4) repeat step 1) -3) 3 times；
(4) soft bag is taken out from ultra high pressure extraction device, pours out material, it is filtered, centrifuge, concentration, produced after drying
Otoginsenoside extract.
Through measuring and calculating, extract yield 16.9%, otoginsenoside purity is 46.6%, the otoginsenoside rate of transform 97.0%.
Embodiment 6
(1) buckeye is crushed into the powder for 100 mesh granularities, is pulled out after soaking 0.5 hour, drain the water on surface
Point, it is placed in household freezer and freezes rapidly；
(2) buckeye after freezing is dried in vacuo, controls the vacuum of drying process in the range of 10~20pa,
Temperature is in the range of 10-50 DEG C；
(3) 10% ethanol of 10 times of weight is added into dried buckeye, is fitted into together in pressure-resistant, flexible soft bag
Sealing, is then placed in the extraction vessel of ultra high pressure extraction device, is extracted at normal temperatures, extraction step is as follows：
1) boost phase：The pressure in extraction vessel is increased to 300Mpa in 20min；
2) packing stage：Keep pressure 15min；
3) the pressure release stage：Pressure is let out as normal pressure rapidly in 15s；
4) repeat step 1) -3) 1 time；
(4) soft bag is taken out from ultra high pressure extraction device, pours out material, it is filtered, centrifuge, concentration, produced after drying
Otoginsenoside extract.
Through measuring and calculating, extract yield 17.3%, otoginsenoside purity is 46.1%, the otoginsenoside rate of transform 98.2%.
Test example
Take and belong to embodiment 1-6 with a batch of medicinal material (content of otoginsenoside is 8.12% in medicinal material), according to not
Same mode is extracted, and Extraction solvent uses 20% ethanol in addition to water boiling and extraction, and extracting method uses this area ripe
The conventional method known.
Prepare following comparative example simultaneously：
Buckeye is crushed into the powder for 15 mesh granularities, adds 20% ethanol of 12 times of weight, immersion fills together after 1 hour
Enter and sealed in pressure-resistant, flexible soft bag, be then placed in the extraction vessel of ultra high pressure extraction device, extracted at normal temperatures,
Extraction step is as follows：
1) boost phase：The pressure in extraction vessel is increased to 200Mpa in 15min；
2) packing stage：Keep pressure 15min；
3) the pressure release stage：Pressure is let out as normal pressure rapidly in 10s；
4) repeat step 1) -3) 1 time；
5) soft bag is taken out from extraction vessel, pours out material, it is filtered, high speed centrifugation, it is concentrated under reduced pressure, after vacuum drying
Produce otoginsenoside extract.
Extract solution is concentrated, calculates extract yield after drying, while detects otoginsenoside content, and according to medicinal material content
The otoginsenoside rate of transform (referring to the ratio that otoginsenoside gross mass in extract accounts for otoginsenoside gross mass in medicinal material) is calculated, as a result
It see the table below.
| Extract yield (%) | Otoginsenoside content (%) | The otoginsenoside rate of transform (%) | |
| Ultrasonic extraction | 16.7 | 38.7 | 79.6 |
| Microwave Extraction | 17.2 | 42.3 | 89.6 |
| Seepage is extracted | 13.5 | 45.2 | 75.1 |
| Circumfluence distillation | 17.2 | 40.3 | 85.4 |
| Supercritical carbon dioxide extracting | 11.3 | 47.0 | 65.4 |
| Water boiling and extraction | 16.0 | 36.4 | 71.7 |
| Comparative example | 17.2 | 45.0 | 95.3 |
As can be seen from the above data, using ultra high pressure extraction, otoginsenoside content and the rate of transform in obtained extract
Obviously higher than extracting methods such as existing ultrasound, microwave, seepages；Simultaneously it is also seen that buckeye medicinal material is freeze-dried
After processing, otoginsenoside content and the rate of transform are above not carrying out the comparative example of freeze-drying process in the product of extraction.Contrast
Example is to further improve extraction effect, it is necessary to which elevated pressure, shortening venting duration, increase extraction time, so as to increase energy consumption
And cost.
Claims (8)
- A kind of 1. method based on freeze-drying ultra high pressure extraction otoginsenoside from buckeye, it is characterised in that including following step Suddenly：(1) buckeye is crushed into the powder for 5-100 mesh granularities, is pulled out after soaking 0.5-3 hours, drain the water on surface Point, it is placed in household freezer and freezes rapidly；(2) buckeye after freezing is dried in vacuo, controls the vacuum of drying process in the range of 10-20pa, temperature In the range of 10-50 DEG C；(3) Extraction solvent of 5-20 times of weight is added into dried buckeye, is fitted into together close in pressure-resistant, flexible soft bag Envelope, is then placed in the extraction vessel of ultra high pressure extraction device, is extracted at normal temperatures, extraction step is as follows：1) boost phase：The pressure in extraction vessel is increased to 100-400Mpa in 5-30min；2) packing stage：Keep pressure 5-20min；3) the pressure release stage：Pressure is let out as normal pressure rapidly in 5-30s；4) repeat step 1) -3) 1-3 times；(4) soft bag is taken out from ultra high pressure extraction device, pours out material, it is filtered, centrifuge, concentration, seven leaves are produced after drying Saponin extract.
- 2. the method as claimed in claim 1 based on freeze-drying ultra high pressure extraction otoginsenoside from buckeye, its feature exist In：The Extraction solvent is water or 10-50% ethanol.
- 3. the method as claimed in claim 1 based on freeze-drying ultra high pressure extraction otoginsenoside from buckeye, its feature exist In：The granularity of the Buckeye Seed is 10-30 mesh.
- 4. the method as claimed in claim 1 based on freeze-drying ultra high pressure extraction otoginsenoside from buckeye, its feature exist In：The Extraction solvent is 10-15 times of buckeye weight.
- 5. the method as claimed in claim 1 based on freeze-drying ultra high pressure extraction otoginsenoside from buckeye, its feature exist In：The boost phase is that the pressure in extraction vessel is increased into 200-300Mpa in 10-15min.
- 6. the method as claimed in claim 1 based on freeze-drying ultra high pressure extraction otoginsenoside from buckeye, its feature exist In：The time of the packing stage is 10-15min.
- 7. the method as claimed in claim 1 based on freeze-drying ultra high pressure extraction otoginsenoside from buckeye, its feature exist In：The time in the pressure release stage is 10-15s.
- 8. the method as claimed in claim 1 based on freeze-drying ultra high pressure extraction otoginsenoside from buckeye, its feature exist In：Repeat step 1) -3) 1 time.
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Cited By (2)
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| CN108497242A (en) * | 2018-04-16 | 2018-09-07 | 恩施土家族苗族自治州农业科学院 | Selenium-rich blue or green money willow health beverages and preparation method thereof |
| CN108929357A (en) * | 2018-08-14 | 2018-12-04 | 安徽弘腾药业有限公司 | A method of quickly extracting Astragaloside IV from Radix Astragali |
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| CN108929357B (en) * | 2018-08-14 | 2021-05-07 | 安徽弘腾药业有限公司 | Method for rapidly extracting astragaloside from astragalus |
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