CN110693927A - Preparation method of horse chestnut extract - Google Patents
Preparation method of horse chestnut extract Download PDFInfo
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- A61K2236/50—Methods involving additional extraction steps
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Abstract
A method for preparing horse chestnut extract comprises the following steps: preparing horse chestnut powder; extracting; spray drying; storing; through the steps, the horse chestnut seeds are crushed, ethanol and acetic acid are used as solvents, the extraction step of the horse chestnut seed extract is completed within 165min in a pressurizing and normal pressure segmented extraction mode, the extraction rate of the active ingredient aescin is improved to over 75% through detection, and meanwhile, microcrystalline cellulose is added and packaged and stored in a vacuumizing mode, so that on one hand, the drying of the horse chestnut extract powder can be kept, and on the other hand, the subsequent application of the horse chestnut extract powder is not influenced.
Description
Technical Field
The invention relates to the technical field of extraction, and particularly relates to a preparation method of a horse chestnut extract.
Background
Horse chestnut trees are deciduous trees and are distributed in European deciduous forest lands. One of the four street trees in the world. The tree body is tall and tall, the crown is wide, the shade is thick, the inflorescence is beautiful, and the tree is widely used as a street tree and a garden ornamental tree in Europe and America.
Aescin extracted from horse chestnut seed is one excellent medicine with the functions of reducing capillary permeability, diminishing inflammation, resisting exudation, protecting vein, raising vein elasticity and tension, promoting vein and lymph reflux, improving microcirculation and resisting oxygen radical.
The existing horse chestnut seed extract is mainly extracted by a fermentation mode, the components in the extract are complex, the extraction time is long, the extraction rate of the effective component aescin can be improved to 65 percent if the extract is fermented for more than 7 days, the extraction efficiency is low, and the cost is high.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a preparation method of a horse chestnut extract, namely, the extraction of the horse chestnut seed extract is completed in a short time by adopting ethanol and acetic acid as solvents and adopting a mode of combining pressurization and normal pressure extraction, and the extraction rate of an effective component aescin is improved to more than 75%.
The invention provides a preparation method of a horse chestnut extract, which comprises the following steps:
preparing horse chestnut powder: pulverizing horse chestnut seeds dried at 0 deg.C to obtain horse chestnut powder with particle size of 80-150 mesh;
extraction: extracting horse chestnut powder by using a mixed solution of ethanol, acetic acid and water, wherein the volume content of the ethanol is 50-70%, the volume content of the acetic acid is 2-5%, 1g of horse chestnut powder is extracted by using 8-15 ml of the mixed solution, the extraction comprises a first extraction stage and a second extraction stage, the first extraction stage is under the conditions that the extraction pressure is 3 atm, the extraction temperature is 60 ℃, the extraction time is kept for 10-15 min, the second extraction stage is under the conditions that the extraction pressure is 1 atm, the extraction temperature is 25 ℃, and the extraction time is kept for 80-150 min;
and (3) suction filtration: carrying out suction filtration on the extracted mixture to obtain a filter cake and a filtrate;
spray drying: spray drying the filtrate to obtain horse chestnut extract powder with water content not higher than 3%;
and (3) storage: adding microcrystalline cellulose with the mass ratio of 5-10% into the horse chestnut extract powder, and performing vacuum packaging and storage.
Further, in the extraction step, ultrasonic-assisted extraction is performed in the first extraction stage and the second extraction stage, wherein the ultrasonic frequency is 35kHz, and the power is 500W.
Further, performing secondary extraction on the filter cake obtained in the suction filtration step, wherein mixed solution of ethanol, acetic acid and water is used for extracting horse chestnut powder in the secondary extraction, 8ml-15ml of mixed solution is used for extracting 1g of filter cake, the volume content of ethanol is 50% -70%, the volume content of acetic acid is 2% -5%, the extraction pressure is 1 atmosphere, the extraction temperature is 25 ℃, and the extraction time is kept for 80min-150 min.
Furthermore, ultrasonic-assisted extraction is adopted during the secondary extraction, the frequency of ultrasonic waves is 35kHz, and the power is 500W.
Further, the mixture obtained by the secondary extraction is filtered by suction, and the filtrate is sprayed and dried to obtain horse chestnut extract powder.
Further, in the preservation step, chitin powder is added into the horse chestnut extract powder, and the mass proportion of the chitin powder is 0.1-0.5%.
Further, in the suction filtration step, the precision of the filter paper adopted by the suction filtration is 0.2-0.5 μm.
Further, in the spray drying step, the temperature of the spray drying is 25-50 ℃.
Further, in the step of preserving, the microcrystalline cellulose has a particle size of 0.1 μm to 1 μm.
Further, in the step of preserving, the crystallinity of the microcrystalline cellulose is 65% to 75%.
Through the steps, the horse chestnut seeds are crushed, ethanol and acetic acid are used as solvents, the extraction step of the horse chestnut seed extract is completed within 165min in a pressurized and normal-pressure segmented extraction mode, and the extraction rate of the effective component aescin is improved to over 75 percent through detection.
In addition, horse chestnut extract powder is obtained by a spray drying mode, microcrystalline cellulose is added, and the horse chestnut extract powder is packaged and stored in a vacuumizing mode.
Detailed Description
The technical solutions of the present invention will be described in detail with reference to specific embodiments, it should be understood that these embodiments are only used for illustrating the present invention and not for limiting the scope of the present invention, and after reading the present invention, the skilled person will modify the present invention in various equivalent forms within the scope defined by the claims appended to the present application.
Example 1
The invention provides a preparation method of a horse chestnut extract, which comprises the following steps:
preparing horse chestnut powder: pulverizing horse chestnut seeds dried at 0 deg.C to obtain horse chestnut powder with particle size of 80-150 mesh;
extraction: extracting horse chestnut powder by using a mixed solution of ethanol, acetic acid and water, wherein the volume content of the ethanol is 50-70%, the volume content of the acetic acid is 2-5%, 1g of horse chestnut powder is extracted by using 8-15 ml of the mixed solution, the extraction comprises a first extraction stage and a second extraction stage, the first extraction stage is under the conditions that the extraction pressure is 3 atm, the extraction temperature is 60 ℃, the extraction time is kept for 10-15 min, the second extraction stage is under the conditions that the extraction pressure is 1 atm, the extraction temperature is 25 ℃, the extraction time is kept for 80-150 min, and ultrasonic auxiliary extraction is carried out in the first extraction stage and the second extraction stage, the ultrasonic frequency is 35kHz, and the power is 500W;
and (3) suction filtration: carrying out suction filtration on the extracted mixture to obtain a filter cake and a filtrate;
in order to further extract a horse chestnut seed extract, performing secondary extraction on the filter cake obtained in the suction filtration step, wherein the secondary extraction adopts mixed solution of ethanol, acetic acid and water to extract horse chestnut powder, 1g of the filter cake is extracted by 8ml-15ml of mixed solution, the volume content of ethanol is 50% -70%, the volume content of acetic acid is 2% -5%, the extraction pressure is 1 atmosphere, the extraction temperature is 25 ℃, the extraction time is kept for 80min-150min, and the secondary extraction is performed by adopting ultrasonic auxiliary extraction, wherein the ultrasonic frequency is 35kHz, and the power is 500W.
Performing suction filtration on the mixture obtained by the secondary extraction, and performing spray drying on the filtrate to obtain horse chestnut extract powder;
spray drying: spray drying the filtrate to obtain horse chestnut extract powder with water content not higher than 3%;
and (3) storage: adding microcrystalline cellulose with the mass ratio of 5-10% into the horse chestnut extract powder, carrying out vacuum packaging and storage, and carrying out vacuum packaging and storage, wherein in the storage step, chitin powder is added into the horse chestnut extract powder, and the addition mass ratio is 0.1-0.5%.
Further, in the preservation step, chitin powder is added into the horse chestnut extract powder, and the mass proportion of the chitin powder is 0.1-0.5%.
Further, in the suction filtration step, the precision of the filter paper adopted by the suction filtration is 0.2-0.5 μm.
Further, in the spray drying step, the temperature of the spray drying is 25-50 ℃.
Further, in the step of preserving, the microcrystalline cellulose has a particle size of 0.1 μm to 1 μm.
Further, in the step of preserving, the crystallinity of the microcrystalline cellulose is 65% to 75%.
In the extraction step, the volume of the mixed solution used for 1g of horse chestnut powder is inversely related to the extraction time, namely, if the volume of the mixed solution used for 1g of horse chestnut powder is X and the extraction time in the second stage is Y, then Y is kX + b, wherein k is a negative number, and the specific experimental results are shown in the following table.
Through the steps, the horse chestnut seeds are crushed, ethanol and acetic acid are used as solvents, the extraction step of the horse chestnut seed extract is completed within 165min in a pressurized and normal-pressure segmented extraction mode, and the extraction rate of the effective component aescin is improved to over 75 percent through detection.
In addition, horse chestnut extract powder is obtained by a spray drying mode, microcrystalline cellulose is added, and the horse chestnut extract powder is packaged and stored in a vacuumizing mode.
The ultrasonic extraction process has high extraction efficiency, and the extraction rate of aescin is generally improved by 3-5%, for example, on the basis of experiment 1, the extraction rate of aescin is improved to 81.5% by ultrasonic-assisted extraction.
In the preservation step, 0.1-0.5% of chitin powder is added, and the chitin powder has natural antibacterial performance, so that the horse chestnut extract powder is not polluted, and the drug effect of the horse chestnut extract is not influenced, so that the preservation period of the horse chestnut extract powder is longer.
Example 2
The invention provides a preparation method of a horse chestnut extract, which comprises the following steps:
preparing horse chestnut powder: pulverizing horse chestnut seeds dried at 0 deg.C to obtain horse chestnut powder with particle size of 100 mesh;
extraction: extracting horse chestnut powder by using a mixed solution of ethanol, acetic acid and water, wherein the volume content of the ethanol is 60%, the volume content of the acetic acid is 3%, 1g of horse chestnut powder is extracted by using 10ml of the mixed solution, the extraction comprises a first extraction stage and a second extraction stage, the first extraction stage is under the conditions that the extraction pressure is 3 atm, the extraction temperature is 60 ℃, the extraction time is kept for 12min, the second extraction stage is under the conditions that the extraction pressure is 1 atm, the extraction temperature is 25 ℃, the extraction time is kept for 100min, and ultrasonic auxiliary extraction is performed in the first extraction stage and the second extraction stage, the ultrasonic frequency is 35kHz, and the power is 500W;
and (3) suction filtration: carrying out suction filtration on the extracted mixture to obtain a filter cake and a filtrate;
in order to further extract a horse chestnut seed extract, performing secondary extraction on the filter cake obtained in the suction filtration step, wherein the secondary extraction adopts a mixed solution of ethanol, acetic acid and water to extract horse chestnut powder, 1g of the filter cake is extracted by 12ml of the mixed solution, the volume content of the ethanol is 60%, the volume content of the acetic acid is 3%, the extraction pressure is 1 atmosphere, the extraction temperature is 25 ℃, the extraction time is kept for 100min, and the secondary extraction adopts ultrasonic auxiliary extraction, wherein the ultrasonic frequency is 35kHz, and the power is 500W.
Performing suction filtration on the mixture obtained by the secondary extraction, and performing spray drying on the filtrate to obtain horse chestnut extract powder;
spray drying: spray drying the filtrate to obtain horse chestnut extract powder with water content not higher than 3%;
and (3) storage: adding microcrystalline cellulose with the mass ratio of 7% into horse chestnut extract powder, vacuum packaging and storing, and in the step of storing, adding chitin powder into horse chestnut extract powder with the mass ratio of 0.3%.
Further, in the suction filtration step, the precision of the filter paper adopted by the suction filtration is 0.3 μm.
Further, in the spray drying step, the temperature at the time of the spray drying was 40 ℃.
Further, in the step of preserving, the microcrystalline cellulose has a particle size of 0.5 μm.
Further, in the step of preserving, the microcrystalline cellulose has a crystallinity of 70%.
Through the steps, the horse chestnut seeds are crushed, ethanol and acetic acid are used as solvents, the extraction step of the horse chestnut seed extract is completed within 112min in a pressurized and normal-pressure segmented extraction mode, and the extraction rate of the effective component aescin is improved to 78.2% through detection.
In addition, horse chestnut extract powder is obtained by a spray drying mode, microcrystalline cellulose is added, and the horse chestnut extract powder is packaged and stored in a vacuumizing mode.
Through the ultrasonic step, the extraction efficiency is high, and the extraction rate of the aescin is generally improved by 3-5 percent, for example, on the basis of the experiment of the embodiment, the extraction rate of the aescin is improved to 81.5 percent through ultrasonic-assisted extraction.
In the preservation step, 0.3% of chitin powder is added, and the chitin powder has natural antibacterial performance, so that horse chestnut extract powder is not polluted, and the drug effect of the horse chestnut extract is not influenced, so that the preservation period of the horse chestnut extract powder is longer.
Example 3
The invention provides a preparation method of a horse chestnut extract, which comprises the following steps:
preparing horse chestnut powder: pulverizing horse chestnut seeds dried at 0 deg.C to obtain horse chestnut powder with particle size of 80 mesh;
extraction: extracting horse chestnut powder by using a mixed solution of ethanol, acetic acid and water, wherein the volume content of the ethanol is 70%, the volume content of the acetic acid is 2%, 1g of the horse chestnut powder is extracted by using 8ml of the mixed solution, the extraction comprises a first extraction stage and a second extraction stage, the first extraction stage is under the conditions that the extraction pressure is 3 atm, the extraction temperature is 60 ℃, the extraction time is kept for 15min, the second extraction stage is under the conditions that the extraction pressure is 1 atm, the extraction temperature is 25 ℃, the extraction time is kept for 80min, and ultrasonic auxiliary extraction is performed in the first extraction stage and the second extraction stage, the ultrasonic frequency is 35kHz, and the power is 500W;
and (3) suction filtration: carrying out suction filtration on the extracted mixture to obtain a filter cake and a filtrate;
in order to further extract a horse chestnut seed extract, performing secondary extraction on the filter cake obtained in the suction filtration step, wherein the secondary extraction adopts a mixed solution of ethanol, acetic acid and water to extract horse chestnut powder, 1g of the filter cake is extracted by 15ml of the mixed solution, the volume content of ethanol is 70%, the volume content of acetic acid is 5%, the extraction pressure is 1 atmosphere, the extraction temperature is 25 ℃, the extraction time is kept for 150min, and the secondary extraction adopts ultrasonic auxiliary extraction, wherein the ultrasonic frequency is 35kHz, and the power is 500W.
Performing suction filtration on the mixture obtained by the secondary extraction, and performing spray drying on the filtrate to obtain horse chestnut extract powder;
spray drying: spray drying the filtrate to obtain horse chestnut extract powder with water content not higher than 3%;
and (3) storage: adding microcrystalline cellulose with the mass ratio of 5% into horse chestnut extract powder, vacuum packaging and storing, and in the step of storing, adding chitin powder into horse chestnut extract powder with the mass ratio of 0.5%.
Further, in the suction filtration step, the precision of the filter paper adopted by the suction filtration is 0.5 μm.
Further, in the spray drying step, the temperature at the time of the spray drying was 50 ℃.
Further, in the step of preserving, the microcrystalline cellulose has a particle size of 1 μm.
Further, in the step of preserving, the microcrystalline cellulose has a crystallinity of 75%.
Through the steps, the horse chestnut seeds are crushed, ethanol and acetic acid are used as solvents, the extraction step of the horse chestnut seed extract is completed in 95min in a pressurized and normal-pressure segmented extraction mode, and the extraction rate of the effective component aescin is improved to 78.8% through detection.
In addition, horse chestnut extract powder is obtained by a spray drying mode, microcrystalline cellulose is added, and the horse chestnut extract powder is packaged and stored in a vacuumizing mode.
The ultrasonic extraction process has high extraction efficiency, and the extraction rate of aescin is improved by 3-5%, for example, on the basis of experiment 1, the extraction rate of aescin is improved to 82.6% by ultrasonic-assisted extraction.
In the preservation step, 0.5% of chitin powder is added, and the chitin powder has natural antibacterial performance, so that horse chestnut extract powder is not polluted, and the drug effect of the horse chestnut extract is not influenced, so that the preservation period of the horse chestnut extract powder is longer.
Claims (10)
1. The preparation method of the horse chestnut extract is characterized by comprising the following steps:
preparing horse chestnut powder: pulverizing horse chestnut seeds dried at 0 deg.C to obtain horse chestnut powder with particle size of 80-150 mesh;
extraction: extracting horse chestnut powder by using a mixed solution of ethanol, acetic acid and water, wherein the volume content of the ethanol is 50-70%, the volume content of the acetic acid is 2-5%, 1g of horse chestnut powder is extracted by using 8-15 ml of the mixed solution, the extraction comprises a first extraction stage and a second extraction stage, the first extraction stage is under the conditions that the extraction pressure is 3 atm, the extraction temperature is 60 ℃, the extraction time is kept for 10-15 min, the second extraction stage is under the conditions that the extraction pressure is 1 atm, the extraction temperature is 25 ℃, and the extraction time is kept for 80-150 min;
and (3) suction filtration: carrying out suction filtration on the extracted mixture to obtain a filter cake and a filtrate;
spray drying: spray drying the filtrate to obtain horse chestnut extract powder with water content not higher than 3%;
and (3) storage: adding microcrystalline cellulose with the mass ratio of 5-10% into the horse chestnut extract powder, and performing vacuum packaging and storage.
2. The method for preparing a horse chestnut extract according to claim 1, wherein in the extraction step, ultrasonic-assisted extraction is performed in the first extraction stage and the second extraction stage, the ultrasonic frequency is 35kHz, and the power is 500W.
3. The method for preparing a horse chestnut extract according to claim 1, characterized in that the filter cake obtained in the suction filtration step is subjected to secondary extraction, the secondary extraction is used for extracting horse chestnut powder by using a mixed solution of ethanol, acetic acid and water, 1g of the filter cake is extracted by using 8ml to 15ml of the mixed solution, the volume content of ethanol is 50 percent to 70 percent, the volume content of acetic acid is 2 percent to 5 percent, the extraction pressure is 1 atmosphere, the extraction temperature is 25 ℃, and the extraction time is kept for 80min to 150 min.
4. A method for preparing horse chestnut extract according to claim 3, characterized in that, the secondary extraction is carried out by ultrasonic assisted extraction, the frequency of the ultrasonic is 35kHz, and the power is 500W.
5. A method for preparing horse chestnut extract according to claim 3, characterized in that the mixture obtained by the secondary extraction is filtered with suction and the filtrate is spray dried to obtain horse chestnut extract powder.
6. The method for preparing a horse chestnut extract according to claim 1, characterized in that in the preservation step, chitin powder is added to the horse chestnut extract powder, and the addition mass ratio is 0.1% -0.5%.
7. A method for preparing horse chestnut extract according to claim 1, characterized in that, in the suction filtration step, the precision of the filter paper used in the suction filtration is 0.2 μm to 0.5 μm.
8. A method of preparing a horse chestnut extract according to claim 1, characterized in that, in the step of spray drying, the temperature of the spray drying is 25 ℃ to 50 ℃.
9. A method for producing a horse chestnut extract according to claim 1, characterized in that, in the preservation step, the microcrystalline cellulose has a particle size of 0.1 μm to 1 μm.
10. A process for the preparation of a horse chestnut extract according to claim 1, characterized in that in the preservation step, the microcrystalline cellulose has a crystallinity of 65% to 75%.
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Citations (5)
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| CN101967175A (en) * | 2010-06-28 | 2011-02-09 | 南京泽朗医药科技有限公司 | Ultrasonic wave-microwave synergetic extraction method for aescine |
| CN102006879A (en) * | 2008-02-13 | 2011-04-06 | 花王株式会社 | Method for producing hippocastanaceae plant seed extract |
| CN107496472A (en) * | 2017-08-07 | 2017-12-22 | 武汉爱民制药股份有限公司 | A kind of method of ultra high pressure extraction otoginsenoside |
| CN107890439A (en) * | 2017-11-15 | 2018-04-10 | 惠州兆骐礼品有限公司 | A kind of extracting method and its hair-washing composition of European horse-chestnut seed extract |
| CN109096351A (en) * | 2018-08-30 | 2018-12-28 | 佛山市欧若拉生物科技有限公司 | A kind of buckeye saponin extraction technique |
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2019
- 2019-11-27 CN CN201911177813.7A patent/CN110693927A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102006879A (en) * | 2008-02-13 | 2011-04-06 | 花王株式会社 | Method for producing hippocastanaceae plant seed extract |
| CN101967175A (en) * | 2010-06-28 | 2011-02-09 | 南京泽朗医药科技有限公司 | Ultrasonic wave-microwave synergetic extraction method for aescine |
| CN107496472A (en) * | 2017-08-07 | 2017-12-22 | 武汉爱民制药股份有限公司 | A kind of method of ultra high pressure extraction otoginsenoside |
| CN107890439A (en) * | 2017-11-15 | 2018-04-10 | 惠州兆骐礼品有限公司 | A kind of extracting method and its hair-washing composition of European horse-chestnut seed extract |
| CN109096351A (en) * | 2018-08-30 | 2018-12-28 | 佛山市欧若拉生物科技有限公司 | A kind of buckeye saponin extraction technique |
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Inventor after: Liu Tingfu Inventor after: Liu Kaihao Inventor after: Shen Yanjun Inventor after: Gu Guanyu Inventor before: Liu Tingfu |