CN106478748A - The method that vacuum and low temperature extracts Folium Sennae effective ingredient - Google Patents
The method that vacuum and low temperature extracts Folium Sennae effective ingredient Download PDFInfo
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- CN106478748A CN106478748A CN201610777978.8A CN201610777978A CN106478748A CN 106478748 A CN106478748 A CN 106478748A CN 201610777978 A CN201610777978 A CN 201610777978A CN 106478748 A CN106478748 A CN 106478748A
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- vacuum
- extract
- folium sennae
- low temperature
- effective ingredient
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/24—Condensed ring systems having three or more rings
- C07H15/244—Anthraquinone radicals, e.g. sennosides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
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- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Medicines Containing Plant Substances (AREA)
- Cosmetics (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a kind of method that vacuum and low temperature extracts Folium Sennae effective ingredient, comprise the steps：1）Extract：Take powder in Folium Sennae to be raw material, after adding Extraction solvent, be placed in the airtight extraction vessel that vacuum is 0.05 0.1Mpa and extract 13 times, extract 10 15 minutes every time, extracted every time after the extracting solution obtaining is collected and merge；2）Filter：Add flocculant in described extracting solution, stir, after standing 0.5 2h, supernatant is filtrated to get filtrate through the filter equipped with ultrafiltration filter membrane；3）Concentrate：Described filtrate is placed in and in vacuum evaporator, is concentrated into the fluid extract that relative density is 1.15 1.20g/ml, and the vacuum in vacuum evaporator is 0.08 0.1MPa, temperature is 30 50 DEG C；4）It is dried：Described fluid extract is atomized, through high-pressure spray gun, the microgranule that nebulizes, and is dried in powdery product under 40 50 DEG C of temperature conditionss.Not only shorten extraction time, eliminate the impact to sennoside for the high temperature, and obtained sennoside good stability, and disclosure satisfy that the requirement of industrialization production.
Description
Technical field
The invention belongs in plant effective component extracting technical field, be specifically that a kind of vacuum and low temperature extracts Folium Sennae
The method of effective ingredient.
Background technology
Folium Sennae is the lobule that is dried of leguminous plant leaf Senna fruit or cassia acutifolia Delile leaf, sweet in the mouth, hardship, cold, returns large intestine channel.It is one
Intestinal stasis relieving agent under clinical conventional the rushing down of kind of people doctor, have that the row that purges heat is stagnant, relieving constipation, the function of diuretic, cure mainly accumulation of heat stagnate, constipation abdomen
Bitterly, oedema turgor, is most widely used catharsis agent in current world wide.Count multiple catharsis agent according to German medical analysis
Service condition shows：Account for nearly 40% about with the use of the related catharsis agent based on Folium Sennae, sales volume is rushed down far above other
Agent it is shown that Folium Sennae application popularity and market development prospect.The effective ingredient of senna effect is dianthrone class
Compound, mainly Sennoside A, B, C, D.Sennoside A, B are under the effect of digestive tract various bacteria by different metabolic pathways
It is degraded to different chrysophanic acid anthrones, produce laxative action.
At present, applying wide in actual production is that alcohol extraction is followed the example of and water extraction, but its extraction efficiency is not high, and
How extracting method to be evaluated for evaluation index with single Sennoside A or sennoside B yield, with total sennoside yield estimator relatively
Few, but extraction ratio in different Extraction medium of Sennoside A, B and stability are not quite similar.If emphatically with Sennoside A or kind
Rush down the extraction ratio evaluation of glycosides B, the extraction ratio of sennoside B or Sennoside A and stability will be remarkably decreased.The total sennoside of water extraction
Leaching rate has 86.2-87.2%, but concentration time is long, and thickening temperature is high so that sennoside loss is big；Although alcohol extracting method extraction ratio
Up to 91.2%, but its long soaking time, and the sennoside stability obtaining is bad.Though it is higher that ultrasonic extraction lifts rate,
But reality is also had some limitations in big production.
Content of the invention
In view of this, it is an object of the invention to provide a kind of vacuum and low temperature extract Folium Sennae effective ingredient method, no
Only shorten extraction time, eliminate the impact to sennoside for the high temperature, and obtained sennoside good stability, and can expire
The requirement of sufficient industrialization production.
For reaching above-mentioned purpose, the present invention provides following technical scheme：
A kind of method that vacuum and low temperature extracts Folium Sennae effective ingredient, comprises the steps：
1）Extract：Take powder in Folium Sennae to be raw material, after adding Extraction solvent, be placed in vacuum and carry for the airtight of 0.05-0.1Mpa
Extract 1-3 time in extracting container, extract 10-15 minute every time, extracted every time after the extracting solution obtaining is collected and merge；
2）Filter：Add flocculant in described extracting solution, stir, after standing 0.5-2h, by supernatant through equipped with ultrafiltration
The filter of filter membrane is filtrated to get filtrate；
3）Concentrate：Described filtrate is placed in and in vacuum evaporator, is concentrated into the fluid extract that relative density is 1.15-1.20g/ml, and
Vacuum in vacuum evaporator is 0.08-0.1MPa, and temperature is 30-50 DEG C；
4）It is dried：Described fluid extract is atomized, through high-pressure spray gun, the microgranule that nebulizes, and is dried extremely under 40-50 DEG C of temperature conditionss
In powdery product.
Further, described step 1）In, described Extraction solvent adopts aqueous lower alcohol, the matter of alcohol in described aqueous lower alcohol
Amount concentration is 30%-60%.
Further, described lower alcohol is the alcohols of 1-3 for carbon chain lengths.
Further, described step 1）In, described Extraction solvent adopts the solution of water and ethanol, and the mass concentration of ethanol is
0%-70%.
Further, described step 1）In, the addition of described Extraction solvent is the 15-20 of silty amount in described Folium Sennae
Times.
Further, described flocculant is at least one in chitin, shitosan and sodium alginate.
Further, described step 2）In, the addition quality of described flocculant and described extracting solution mass ratio are 0.02-
0.04%.
Further, described step 2）In, described ultrafiltration filter membrane adopts cellulose acetate membrane, polyamide, polyether sulfone or hollow
Cellulose membrane.
Further, described step 4）In, the granularity of described vaporific microgranule is 200 mesh.
The beneficial effects of the present invention is：
The overall process that vacuum and low temperature of the present invention extracts the method for Folium Sennae effective ingredient all completes at low temperature, not only has Senna fruit
Glycosides loss is few, simple to operate, extracting cycle is short, equipment requirements are not high, the advantage of suitable for scale production and energy-conserving and environment-protective, and
And obtain Senna fruit A, B total glycosides percentage composition and account for crude drug in whole total sennoside more than 90%, obtained stable effective ingredients are good,
It is easy to preserve it can be seen that the method that vacuum and low temperature of the present invention extracts Folium Sennae effective ingredient has significant economic benefit and society
Can benefit.
Specific embodiment
With reference to specific embodiment, the invention will be further described, so that those skilled in the art can be more preferable
Understand the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
Embodiment 1
The method that the present embodiment vacuum and low temperature extracts Folium Sennae effective ingredient, comprises the steps：
1）Extract：Take powder in Folium Sennae to be raw material, after adding Extraction solvent, be placed in the airtight extraction that vacuum is 0.08Mpa and hold
Extract 2 times in device, extract 10 minutes every time, extracted every time after the extracting solution obtaining is collected and merge；The extraction of the present embodiment is molten
The addition of agent is 15 times of silty amount in Folium Sennae, and Extraction solvent adopts aqueous lower alcohol, the matter of alcohol in aqueous lower alcohol
Amount concentration is 30%, and lower alcohol is the alcohols of 1-3 for carbon chain lengths.
2）Filter：Add flocculant in extracting solution, stir, after standing 0.5h, by supernatant through equipped with ultrafiltration filter
The filter of film is filtrated to get filtrate；The addition quality of the flocculant of the present embodiment and extracting solution mass ratio are 0.03%, and wad a quilt with cotton
Solidifying agent is at least one in chitin, shitosan and sodium alginate, and ultrafiltration filter membrane adopts cellulose acetate membrane, polyamide, gathers
Ether sulfone or hollow cellulose film.The flocculant of the present embodiment is chitin, and ultrafiltration filter membrane adopts cellulose acetate membrane.
3）Concentrate：Filtrate is placed in and in vacuum evaporator, is concentrated into the fluid extract that relative density is 1.18g/ml, and vacuum
Vacuum in vaporizer is 0.08MPa, and temperature is 40 DEG C.
4）It is dried：Fluid extract is atomized into the vaporific microgranule of 200 purposes through high-pressure spray gun, and dry under 40 DEG C of temperature conditionss
Dry in powdery product.
The overall process that the present embodiment vacuum and low temperature extracts the method for Folium Sennae effective ingredient all completes at low temperature, not only has
Few, simple to operate, extracting cycle is short, equipment requirements are not high, suitable for scale production and energy-conserving and environment-protective to have sennoside to lose
Advantage, and obtain Senna fruit A, B total glycosides percentage composition and account for crude drug in whole total sennoside more than 90%, obtained stable effective ingredients
Property good it is easy to preserve, the Sennoside A of the present embodiment or extraction ratio of sennoside B is 90.76% it can be seen that vacuum of the present invention
The method of extract at low temperature Folium Sennae effective ingredient has significant economic benefit and social benefit.
Embodiment 2
The method that the present embodiment vacuum and low temperature extracts Folium Sennae effective ingredient, comprises the steps：
1）Extract：Take powder in Folium Sennae to be raw material, after adding Extraction solvent, be placed in the airtight extraction that vacuum is 0.05Mpa and hold
Extract 1 time in device, extract 10 minutes every time, extracted every time after the extracting solution obtaining is collected and merge；The extraction of the present embodiment is molten
The addition of agent is 16 times of silty amount in Folium Sennae, and Extraction solvent adopts aqueous lower alcohol, the matter of alcohol in aqueous lower alcohol
Amount concentration is 60%, and lower alcohol is the alcohols of 1-3 for carbon chain lengths.
2）Filter：Add flocculant in extracting solution, stir, after standing 1h, by supernatant through equipped with ultrafiltration filter membrane
Filter be filtrated to get filtrate；The addition quality of the flocculant of the present embodiment and extracting solution mass ratio are 0.02%, and flocculate
Agent is at least one in chitin, shitosan and sodium alginate, and ultrafiltration filter membrane adopts cellulose acetate membrane, polyamide, polyethers
Sulfone or hollow cellulose film.The flocculant of the present embodiment is the mixture of shitosan and sodium alginate, and ultrafiltration filter membrane adopts hollow
Cellulose membrane.
3）Concentrate：Filtrate is placed in and in vacuum evaporator, is concentrated into the fluid extract that relative density is 1.15g/ml, and vacuum
Vacuum in vaporizer is 0.09MPa, and temperature is 30 DEG C.
4）It is dried：Fluid extract is atomized into the vaporific microgranule of 200 purposes through high-pressure spray gun, and dry under 45 DEG C of temperature conditionss
Dry in powdery product.
The overall process that the present embodiment vacuum and low temperature extracts the method for Folium Sennae effective ingredient all completes at low temperature, not only has
Few, simple to operate, extracting cycle is short, equipment requirements are not high, suitable for scale production and energy-conserving and environment-protective to have sennoside to lose
Advantage, and obtain Senna fruit A, B total glycosides percentage composition and account for crude drug in whole total sennoside more than 90%, obtained stable effective ingredients
Property good it is easy to preserve, the Sennoside A of the present embodiment or extraction ratio of sennoside B is 92.56% it can be seen that vacuum of the present invention
The method of extract at low temperature Folium Sennae effective ingredient has significant economic benefit and social benefit.
Embodiment 3
The method that the present embodiment vacuum and low temperature extracts Folium Sennae effective ingredient, comprises the steps：
1）Extract：Take powder in Folium Sennae to be raw material, after adding Extraction solvent, be placed in the airtight extraction that vacuum is 0.10Mpa and hold
Extract 3 times in device, extract 15 minutes every time, extracted every time after the extracting solution obtaining is collected and merge；The extraction of the present embodiment is molten
The addition of agent is 20 times of silty amount in Folium Sennae, and Extraction solvent adopts aqueous lower alcohol, the matter of alcohol in aqueous lower alcohol
Amount concentration is 40%, and lower alcohol is the alcohols of 1-3 for carbon chain lengths.
2）Filter：Add flocculant in extracting solution, stir, after standing 2h, by supernatant through equipped with ultrafiltration filter membrane
Filter be filtrated to get filtrate；The addition quality of the flocculant of the present embodiment and extracting solution mass ratio are 0.04%, and flocculate
Agent is at least one in chitin, shitosan and sodium alginate, and ultrafiltration filter membrane adopts cellulose acetate membrane, polyamide, polyethers
Sulfone or hollow cellulose film.The flocculant of the present embodiment is sodium alginate, and ultrafiltration filter membrane adopts polyamide.
3）Concentrate：Filtrate is placed in and in vacuum evaporator, is concentrated into the fluid extract that relative density is 1.20g/ml, and vacuum
Vacuum in vaporizer is 0.10MPa, and temperature is 50 DEG C.
4）It is dried：Fluid extract is atomized into the vaporific microgranule of 200 purposes through high-pressure spray gun, and dry under 50 DEG C of temperature conditionss
Dry in powdery product.
The overall process that the present embodiment vacuum and low temperature extracts the method for Folium Sennae effective ingredient all completes at low temperature, not only has
Few, simple to operate, extracting cycle is short, equipment requirements are not high, suitable for scale production and energy-conserving and environment-protective to have sennoside to lose
Advantage, and obtain Senna fruit A, B total glycosides percentage composition and account for crude drug in whole total sennoside more than 90%, obtained stable effective ingredients
Property good it is easy to preserve, the Sennoside A of the present embodiment or extraction ratio of sennoside B is 91.85% it can be seen that vacuum of the present invention
The method of extract at low temperature Folium Sennae effective ingredient has significant economic benefit and social benefit.
Embodiment 4
The method that the present embodiment vacuum and low temperature extracts Folium Sennae effective ingredient, comprises the steps：
1）Extract：Take powder in Folium Sennae to be raw material, after adding Extraction solvent, be placed in the airtight extraction that vacuum is 0.09Mpa and hold
Extract 3 times in device, extract 12 minutes every time, extracted every time after the extracting solution obtaining is collected and merge；The extraction of the present embodiment is molten
The addition of agent is 18 times of silty amount in Folium Sennae, and Extraction solvent adopts the solution of water and ethanol, and the quality of ethanol is dense
Spend for 65%, certainly, the mass concentration of ethanol can also adopt 0%, 12%, 30%, 50% or 70% etc., all disclosure satisfy that using will
Ask, its principle is identical, is not repeated.
2）Filter：Add flocculant in extracting solution, stir, after standing 1.5h, by supernatant through equipped with ultrafiltration filter
The filter of film is filtrated to get filtrate；The addition quality of the flocculant of the present embodiment and extracting solution mass ratio are 0.04%, and wad a quilt with cotton
Solidifying agent is at least one in chitin, shitosan and sodium alginate, and ultrafiltration filter membrane adopts cellulose acetate membrane, polyamide, gathers
Ether sulfone or hollow cellulose film.The flocculant of the present embodiment is chitin, and ultrafiltration filter membrane adopts cellulose acetate membrane.
3）Concentrate：Filtrate is placed in and in vacuum evaporator, is concentrated into the fluid extract that relative density is 1.20g/ml, and vacuum
Vacuum in vaporizer is 0.08MPa, and temperature is 45 DEG C.
4）It is dried：Fluid extract is atomized into the vaporific microgranule of 200 purposes through high-pressure spray gun, and dry under 48 DEG C of temperature conditionss
Dry in powdery product.
The overall process that the present embodiment vacuum and low temperature extracts the method for Folium Sennae effective ingredient all completes at low temperature, not only has
Few, simple to operate, extracting cycle is short, equipment requirements are not high, suitable for scale production and energy-conserving and environment-protective to have sennoside to lose
Advantage, and obtain Senna fruit A, B total glycosides percentage composition and account for crude drug in whole total sennoside more than 90%, obtained stable effective ingredients
Property good it is easy to preserve, the Sennoside A of the present embodiment or extraction ratio of sennoside B is 91.85% it can be seen that vacuum of the present invention
The method of extract at low temperature Folium Sennae effective ingredient has significant economic benefit and social benefit.
Embodiment described above is only the preferred embodiment lifted for absolutely proving the present invention, the protection model of the present invention
Enclose not limited to this.Equivalent substitute or conversion that those skilled in the art are made on the basis of the present invention, all in the present invention
Protection domain within.Protection scope of the present invention is defined by claims.
Claims (9)
1. a kind of vacuum and low temperature extract Folium Sennae effective ingredient method it is characterised in that：Comprise the steps：
1）Extract：Take powder in Folium Sennae to be raw material, after adding Extraction solvent, be placed in vacuum and carry for the airtight of 0.05-0.1Mpa
Extract 1-3 time in extracting container, extract 10-15 minute every time, extracted every time after the extracting solution obtaining is collected and merge；
2）Filter：Add flocculant in described extracting solution, stir, after standing 0.5-2h, by supernatant through equipped with ultrafiltration
The filter of filter membrane is filtrated to get filtrate；
3）Concentrate：Described filtrate is placed in and in vacuum evaporator, is concentrated into the fluid extract that relative density is 1.15-1.20g/ml, and
Vacuum in vacuum evaporator is 0.08-0.1MPa, and temperature is 30-50 DEG C；
4）It is dried：Described fluid extract is atomized, through high-pressure spray gun, the microgranule that nebulizes, and is dried extremely under 40-50 DEG C of temperature conditionss
In powdery product.
2. vacuum and low temperature according to claim 1 extract Folium Sennae effective ingredient method it is characterised in that：Described step
1）In, described Extraction solvent adopts aqueous lower alcohol, and in described aqueous lower alcohol, the mass concentration of alcohol is 30%-60%.
3. vacuum and low temperature according to claim 2 extract Folium Sennae effective ingredient method it is characterised in that：Described rudimentary
Alcohol is the alcohols of 1-3 for carbon chain lengths.
4. vacuum and low temperature according to claim 1 extract Folium Sennae effective ingredient method it is characterised in that：Described step
1）In, described Extraction solvent adopts the solution of water and ethanol, and the mass concentration of ethanol is 0%-70%.
5. vacuum and low temperature according to any one of claim 1-4 extract Folium Sennae effective ingredient method it is characterised in that：
Described step 1）In, the addition of described Extraction solvent is 15-20 times of silty amount in described Folium Sennae.
6. vacuum and low temperature according to claim 1 extract Folium Sennae effective ingredient method it is characterised in that：Described flocculation
Agent is at least one in chitin, shitosan and sodium alginate.
7. vacuum and low temperature according to claim 1 or 6 extract Folium Sennae effective ingredient method it is characterised in that：Described
Step 2）In, the addition quality of described flocculant and described extracting solution mass ratio are 0.02-0.04%.
8. vacuum and low temperature according to claim 1 extract Folium Sennae effective ingredient method it is characterised in that：Described step
2）In, described ultrafiltration filter membrane adopts cellulose acetate membrane, polyamide, polyether sulfone or hollow cellulose film.
9. vacuum and low temperature according to claim 1 extract Folium Sennae effective ingredient method it is characterised in that：Described step
4）In, the granularity of described vaporific microgranule is 200 mesh.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111084795A (en) * | 2019-09-12 | 2020-05-01 | 天津芸熙生物技术有限公司 | Preparation process of compound preparation extracted from sandalwood leaves at low temperature |
| CN115518100A (en) * | 2022-11-24 | 2022-12-27 | 安顺市宝林科技中药饮片有限公司 | Method for extracting effective components of Chinese medicinal material rhubarb |
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| CN102040637A (en) * | 2010-09-27 | 2011-05-04 | 南京泽朗医药科技有限公司 | Method for extracting sennoside |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111084795A (en) * | 2019-09-12 | 2020-05-01 | 天津芸熙生物技术有限公司 | Preparation process of compound preparation extracted from sandalwood leaves at low temperature |
| CN115518100A (en) * | 2022-11-24 | 2022-12-27 | 安顺市宝林科技中药饮片有限公司 | Method for extracting effective components of Chinese medicinal material rhubarb |
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