CN106478748B - The method that vacuum and low temperature extracts folium sennae active ingredient - Google Patents
The method that vacuum and low temperature extracts folium sennae active ingredient Download PDFInfo
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- CN106478748B CN106478748B CN201610777978.8A CN201610777978A CN106478748B CN 106478748 B CN106478748 B CN 106478748B CN 201610777978 A CN201610777978 A CN 201610777978A CN 106478748 B CN106478748 B CN 106478748B
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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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Abstract
The invention discloses a kind of methods that vacuum and low temperature extracts folium sennae active ingredient, include the following steps：1）Extraction：It is raw material to take powder in folium sennae, after Extraction solvent is added, is placed in the closed extraction vessel that vacuum degree is 0.05 0.1Mpa and extracts 13 times, every time extraction 10 15 minutes, will extract after obtained extracting solution is collected and merges every time；2）Filtering：Flocculant is added into the extracting solution, stirs evenly, after standing 0.5 2h, supernatant is passed through into the filter equipped with ultrafiltration filter membrane, filtrate is obtained by filtration；3）Concentration：The filtrate is placed in cold boiler to the liquid extract for being concentrated into that relative density is 1.15 1.20g/ml, and the vacuum degree in cold boiler is 0.08 0.1MPa, temperature is 30 50 DEG C；4）It is dry：The liquid extract is atomized the particle that nebulizes through high-pressure spray gun, and dry in powdery product under 40 50 DEG C of temperature condition.Extraction time is not only shortened, eliminates influence of the high temperature to sennoside, and obtained sennoside stability is good, and disclosure satisfy that the requirement of industrialization production.
Description
Technical field
The invention belongs to the effective component extracting technical fields in plant, specifically extract folium sennae for a kind of vacuum and low temperature
The method of active ingredient.
Background technology
Folium sennae is the drying leaflet of legume leaf cassia angustifolia or cassia acutifolia Delile leaf, sweet in flavor, bitter, cold, returns large intestine channel.It is one
Kind of people doctor is clinically used rush down under lead stagnant dose, the stagnant row that has the function of to purge heat, defaecation, sharp water, cure mainly heat knot stagnate, constipation abdomen
Bitterly, oedema turgor is catharsis agent most widely used in current world wide.A variety of catharsis agent are counted according to German medical analysis
Service condition is shown：Nearly 40% or so is accounted for the use containing the related catharsis agent based on folium sennae, sales volume is rushed down far above other
Agent, it is shown that the popularity and market development foreground of folium sennae application.The active ingredient of senna effect is dianthrone class
Compound, mainly Sennoside A, B, C, D.Sennoside A, B pass through different metabolic pathways under the effect of alimentary canal various bacteria
Different Rhein anthrones are degraded to, laxative action is generated.
Currently, it is that alcohol extracting is followed the example of and water extraction, but its extraction efficiency is not high using wide in actual production, and
Extracting method is mostly evaluated as evaluation index using single Sennoside A or Sennoside B yield, with total sennoside yield estimator compared with
It is few, but the recovery rate and stability of Sennoside A, B in different Extraction mediums are not quite similar.If emphatically with Sennoside A or kind
The recovery rate evaluation of glycosides B is rushed down, the recovery rate and stability of Sennoside B or Sennoside A 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 recovery rate
Reachable 91.2%, but its long soaking time, and obtained sennoside stability is bad.It is higher that though ultrasonic extraction lifts rate,
But for there is also certain limitations in practical big production.
Invention content
In view of this, the purpose of the present invention is to provide a kind of methods that vacuum and low temperature extracts folium sennae active ingredient, no
Extraction time is only shortened, eliminates influence of the high temperature to sennoside, and obtained sennoside stability is good, and can expire
The requirement of sufficient industrialization production.
In order to achieve the above objectives, the present invention provides the following technical solutions：
A kind of method of vacuum and low temperature extraction folium sennae active ingredient, includes the following steps：
1）Extraction：It is raw material to take powder in folium sennae, and after Extraction solvent is added, it is the close of 0.05-0.1Mpa to be placed in vacuum degree
It closes in extraction vessel and extracts 1-3 times, every time extraction 10-15 minutes, will extract after obtained extracting solution is collected and merge every time；
2）Filtering：Flocculant is added into the extracting solution, stirs evenly, after standing 0.5-2h, by supernatant through being equipped with
Filtrate is obtained by filtration in the filter of ultrafiltration filter membrane；
3）Concentration：The filtrate is placed in cold boiler to the stream leaching for being concentrated into that relative density is 1.15-1.20g/ml
Cream, and the vacuum degree in cold boiler is 0.08-0.1MPa, temperature is 30-50 DEG C；
4）It is dry：The liquid extract is atomized the particle that nebulizes through high-pressure spray gun, and is done under 40-50 DEG C of temperature condition
Dry is extremely in powdery product.
Further, the step 1）In, the Extraction solvent uses aqueous lower alcohol, the matter of alcohol in the aqueous lower alcohol
Measure a concentration of 30%-60%.
Further, the lower alcohol is the alcohols that carbon chain lengths are 1-3.
Further, the step 1）In, the Extraction solvent uses the solution of water and ethyl alcohol, and the mass concentration of ethyl alcohol is
0%-70%。
Further, the step 1）In, the addition of the Extraction solvent is the 15-20 of silty amount in the folium sennae
Times.
Further, the flocculant is at least one of chitin, chitosan and sodium alginate.
Further, the step 2）In, the addition quality of the flocculant is 0.02- with the extracting solution mass ratio
0.04%。
Further, the step 2）In, the ultrafiltration filter membrane is using cellulose acetate film, polyamide, polyether sulfone or hollow
Cellulose membrane.
Further, the step 4）In, the granularity of the mist particle is 200 mesh.
The beneficial effects of the present invention are：
The overall process of the method for vacuum and low temperature extraction folium sennae active ingredient of the present invention is completed at low temperature, is not only had
Sennoside loss is few, easy to operate, extracting cycle is short, equipment requirement is not high, suitable for scale production and energy-saving and environment-friendly excellent
Point, and obtain the total glycosides percentage composition of cassia angustifolia A, B and account for 90% or more crude drug in whole total sennoside, obtained stable effective ingredients
Well, it is easy to preserve, it can be seen that the method for vacuum and low temperature extraction folium sennae active ingredient of the present invention has significant economic effect
Benefit and social benefit.
Specific implementation mode
The present invention is further explained in the light of specific embodiments, so that those skilled in the art can be better
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 active ingredient, includes the following steps：
1）Extraction：It is raw material to take powder in folium sennae, and after Extraction solvent is added, it is that the closed of 0.08Mpa carries to be placed in vacuum degree
It is extracted 2 times in extracting container, every time extraction 10 minutes, will extract after obtained extracting solution is collected and merge every time；The present embodiment carries
The addition of solvent is taken to be 15 times of silty amount in folium sennae, and Extraction solvent uses aqueous lower alcohol, alcohol in aqueous lower alcohol
Mass concentration be 30%, and lower alcohol is the alcohols that carbon chain lengths are 1-3.
2）Filtering：Flocculant is added into extracting solution, stirs evenly, after standing 0.5h, supernatant is passed through and is filtered equipped with ultrafiltration
Filtrate is obtained by filtration in the filter of film；The addition quality of the flocculant of the present embodiment is 0.03% with extracting solution mass ratio, and is wadded a quilt with cotton
Solidifying agent is at least one of chitin, chitosan and sodium alginate, and ultrafiltration filter membrane uses cellulose acetate film, polyamide, gathers
Ether sulfone or hollow cellulose film.The flocculant of the present embodiment is chitin, and ultrafiltration filter membrane uses cellulose acetate film.
3）Concentration：Filtrate is placed in cold boiler to the liquid extract for being concentrated into that relative density is 1.18g/ml, and vacuum
Vacuum degree in evaporator is 0.08MPa, and temperature is 40 DEG C.
4）It is dry：Liquid extract is atomized into the misty particle of 200 mesh through high-pressure spray gun, and is done under 40 DEG C of temperature condition
Dry is extremely in powdery product.
The overall process of the method for the present embodiment vacuum and low temperature extraction folium sennae active ingredient is completed at low temperature, is not only had
Having sennoside to lose, few, easy to operate, extracting cycle is short, equipment requirement is not high, suitable for scale production and energy-saving and environment-friendly
Advantage, and obtain the total glycosides percentage composition of cassia angustifolia A, B and account for 90% or more crude drug in whole total sennoside, obtained stable effective ingredients
Property it is good, be easy to preserve, the Sennoside A of the present embodiment or the recovery rate of Sennoside B are 90.76%, it can be seen that vacuum of the present invention
The method that low temperature extracts folium sennae active ingredient has significant economic benefit and social benefit.
Embodiment 2
The method that the present embodiment vacuum and low temperature extracts folium sennae active ingredient, includes the following steps：
1）Extraction：It is raw material to take powder in folium sennae, and after Extraction solvent is added, it is that the closed of 0.05Mpa carries to be placed in vacuum degree
It is extracted 1 time in extracting container, every time extraction 10 minutes, will extract after obtained extracting solution is collected and merge every time；The present embodiment carries
The addition of solvent is taken to be 16 times of silty amount in folium sennae, and Extraction solvent uses aqueous lower alcohol, alcohol in aqueous lower alcohol
Mass concentration be 60%, and lower alcohol is the alcohols that carbon chain lengths are 1-3.
2）Filtering：Flocculant is added into extracting solution, stirs evenly, after standing 1h, supernatant is passed through, ultrafiltration filter membrane is housed
Filter filtrate is obtained by filtration；The addition quality of the flocculant of the present embodiment is 0.02% with extracting solution mass ratio, and is flocculated
Agent is at least one of chitin, chitosan and sodium alginate, and ultrafiltration filter membrane is using cellulose acetate film, polyamide, polyethers
Sulfone or hollow cellulose film.The flocculant of the present embodiment is the mixture of chitosan and sodium alginate, and ultrafiltration filter membrane is using hollow
Cellulose membrane.
3）Concentration：Filtrate is placed in cold boiler to the liquid extract for being concentrated into that relative density is 1.15g/ml, and vacuum
Vacuum degree in evaporator is 0.09MPa, and temperature is 30 DEG C.
4）It is dry：Liquid extract is atomized into the misty particle of 200 mesh through high-pressure spray gun, and is done under 45 DEG C of temperature condition
Dry is extremely in powdery product.
The overall process of the method for the present embodiment vacuum and low temperature extraction folium sennae active ingredient is completed at low temperature, is not only had
Having sennoside to lose, few, easy to operate, extracting cycle is short, equipment requirement is not high, suitable for scale production and energy-saving and environment-friendly
Advantage, and obtain the total glycosides percentage composition of cassia angustifolia A, B and account for 90% or more crude drug in whole total sennoside, obtained stable effective ingredients
Property it is good, be easy to preserve, the Sennoside A of the present embodiment or the recovery rate of Sennoside B are 92.56%, it can be seen that vacuum of the present invention
The method that low temperature extracts folium sennae active ingredient has significant economic benefit and social benefit.
Embodiment 3
The method that the present embodiment vacuum and low temperature extracts folium sennae active ingredient, includes the following steps：
1）Extraction：It is raw material to take powder in folium sennae, and after Extraction solvent is added, it is that the closed of 0.10Mpa carries to be placed in vacuum degree
It is extracted 3 times in extracting container, every time extraction 15 minutes, will extract after obtained extracting solution is collected and merge every time；The present embodiment carries
The addition of solvent is taken to be 20 times of silty amount in folium sennae, and Extraction solvent uses aqueous lower alcohol, alcohol in aqueous lower alcohol
Mass concentration be 40%, and lower alcohol is the alcohols that carbon chain lengths are 1-3.
2）Filtering：Flocculant is added into extracting solution, stirs evenly, after standing 2h, supernatant is passed through, ultrafiltration filter membrane is housed
Filter filtrate is obtained by filtration；The addition quality of the flocculant of the present embodiment is 0.04% with extracting solution mass ratio, and is flocculated
Agent is at least one of chitin, chitosan and sodium alginate, and ultrafiltration filter membrane is using cellulose acetate film, polyamide, polyethers
Sulfone or hollow cellulose film.The flocculant of the present embodiment is sodium alginate, and ultrafiltration filter membrane uses polyamide.
3）Concentration：Filtrate is placed in cold boiler to the liquid extract for being concentrated into that relative density is 1.20g/ml, and vacuum
Vacuum degree in evaporator is 0.10MPa, and temperature is 50 DEG C.
4）It is dry：Liquid extract is atomized into the misty particle of 200 mesh through high-pressure spray gun, and is done under 50 DEG C of temperature condition
Dry is extremely in powdery product.
The overall process of the method for the present embodiment vacuum and low temperature extraction folium sennae active ingredient is completed at low temperature, is not only had
Having sennoside to lose, few, easy to operate, extracting cycle is short, equipment requirement is not high, suitable for scale production and energy-saving and environment-friendly
Advantage, and obtain the total glycosides percentage composition of cassia angustifolia A, B and account for 90% or more crude drug in whole total sennoside, obtained stable effective ingredients
Property it is good, be easy to preserve, the Sennoside A of the present embodiment or the recovery rate of Sennoside B are 91.85%, it can be seen that vacuum of the present invention
The method that low temperature extracts folium sennae active ingredient has significant economic benefit and social benefit.
Embodiment 4
The method that the present embodiment vacuum and low temperature extracts folium sennae active ingredient, includes the following steps：
1）Extraction：It is raw material to take powder in folium sennae, and after Extraction solvent is added, it is that the closed of 0.09Mpa carries to be placed in vacuum degree
It is extracted 3 times in extracting container, every time extraction 12 minutes, will extract after obtained extracting solution is collected and merge every time；The present embodiment carries
It is 18 times of silty amount in folium sennae to take the addition of solvent, and Extraction solvent uses the solution of water and ethyl alcohol, and the matter of ethyl alcohol
A concentration of 65% is measured, certainly, the mass concentration of ethyl alcohol can also use 0%, 12%, 30%, 50% or 70% etc., disclosure satisfy that use
It is required that principle is identical, it is not repeated.
2）Filtering：Flocculant is added into extracting solution, stirs evenly, after standing 1.5h, supernatant is passed through and is filtered equipped with ultrafiltration
Filtrate is obtained by filtration in the filter of film；The addition quality of the flocculant of the present embodiment is 0.04% with extracting solution mass ratio, and is wadded a quilt with cotton
Solidifying agent is at least one of chitin, chitosan and sodium alginate, and ultrafiltration filter membrane uses cellulose acetate film, polyamide, gathers
Ether sulfone or hollow cellulose film.The flocculant of the present embodiment is chitin, and ultrafiltration filter membrane uses cellulose acetate film.
3）Concentration：Filtrate is placed in cold boiler to the liquid extract for being concentrated into that relative density is 1.20g/ml, and vacuum
Vacuum degree in evaporator is 0.08MPa, and temperature is 45 DEG C.
4）It is dry：Liquid extract is atomized into the misty particle of 200 mesh through high-pressure spray gun, and is done under 48 DEG C of temperature condition
Dry is extremely in powdery product.
The overall process of the method for the present embodiment vacuum and low temperature extraction folium sennae active ingredient is completed at low temperature, is not only had
Having sennoside to lose, few, easy to operate, extracting cycle is short, equipment requirement is not high, suitable for scale production and energy-saving and environment-friendly
Advantage, and obtain the total glycosides percentage composition of cassia angustifolia A, B and account for 90% or more crude drug in whole total sennoside, obtained stable effective ingredients
Property it is good, be easy to preserve, the Sennoside A of the present embodiment or the recovery rate of Sennoside B are 91.85%, it can be seen that vacuum of the present invention
The method that low temperature extracts folium sennae active ingredient has significant economic benefit and social benefit.
Embodiment described above is only to absolutely prove preferred embodiment that is of the invention and being lifted, protection model of the invention
It encloses without being limited thereto.Those skilled in the art on the basis of the present invention made by equivalent substitute or transformation, in the present invention
Protection domain within.Protection scope of the present invention is subject to claims.
Claims (12)
1. a kind of method of vacuum and low temperature extraction folium sennae active ingredient, it is characterised in that：Include the following steps：
1）Extraction：It is raw material to take powder in folium sennae, and after Extraction solvent is added, it is that the closed of 0.05-0.1Mpa carries to be placed in vacuum degree
It is extracted 1-3 times in extracting container, every time extraction 10-15 minutes, will extract after obtained extracting solution is collected and merge every time；The extraction
Solvent uses aqueous lower alcohol, and the mass concentration of alcohol is 30%-60% in the aqueous lower alcohol；The lower alcohol is carbon chain lengths
For the alcohols of 1-3；
2）Filtering：Flocculant is added into the extracting solution, stirs evenly, after standing 0.5-2h, supernatant is passed through, ultrafiltration is housed
Filtrate is obtained by filtration in the filter of filter membrane；
3）Concentration：The filtrate is placed in cold boiler to the liquid extract for being concentrated into that relative density is 1.15-1.20g/ml, and
Vacuum degree in cold boiler is 0.08-0.1MPa, and temperature is 30-50 DEG C；
4）It is dry：The liquid extract is atomized the particle that nebulizes through high-pressure spray gun, and is dried extremely under 40-50 DEG C of temperature condition
In powdery product.
2. the method for vacuum and low temperature extraction folium sennae active ingredient according to claim 1, it is characterised in that：The step
1）In, the addition of the Extraction solvent is 15-20 times of silty amount in the folium sennae.
3. the method for vacuum and low temperature extraction folium sennae active ingredient according to claim 1, it is characterised in that：The flocculation
Agent is at least one of chitin, chitosan and sodium alginate.
4. the method for vacuum and low temperature extraction folium sennae active ingredient according to claim 1 or 3, it is characterised in that：It is described
Step 2）In, the addition quality of the flocculant is 0.02-0.04% with the extracting solution mass ratio.
5. the method for vacuum and low temperature extraction folium sennae active ingredient according to claim 1, it is characterised in that：The step
2）In, the ultrafiltration filter membrane uses cellulose acetate film, polyamide, polyether sulfone or hollow cellulose film.
6. the method for vacuum and low temperature extraction folium sennae active ingredient according to claim 1, it is characterised in that：The step
4）In, the granularity of the mist particle is 200 mesh.
7. a kind of method of vacuum and low temperature extraction folium sennae active ingredient, it is characterised in that：Include the following steps：
1）Extraction：It is raw material to take powder in folium sennae, and after Extraction solvent is added, it is that the closed of 0.05-0.1Mpa carries to be placed in vacuum degree
It is extracted 1-3 times in extracting container, every time extraction 10-15 minutes, will extract after obtained extracting solution is collected and merge every time；The extraction
Solvent uses the solution of water and ethyl alcohol, and the mass concentration of ethyl alcohol is 12%-70%；
2）Filtering：Flocculant is added into the extracting solution, stirs evenly, after standing 0.5-2h, supernatant is passed through, ultrafiltration is housed
Filtrate is obtained by filtration in the filter of filter membrane；
3）Concentration：The filtrate is placed in cold boiler to the liquid extract for being concentrated into that relative density is 1.15-1.20g/ml, and
Vacuum degree in cold boiler is 0.08-0.1MPa, and temperature is 30-50 DEG C；
4）It is dry：The liquid extract is atomized the particle that nebulizes through high-pressure spray gun, and is dried extremely under 40-50 DEG C of temperature condition
In powdery product.
8. the method for vacuum and low temperature extraction folium sennae active ingredient according to claim 7, it is characterised in that：The step
1）In, the addition of the Extraction solvent is 15-20 times of silty amount in the folium sennae.
9. the method for vacuum and low temperature extraction folium sennae active ingredient according to claim 7, it is characterised in that：The flocculation
Agent is at least one of chitin, chitosan and sodium alginate.
10. the method for the vacuum and low temperature extraction folium sennae active ingredient according to claim 7 or 9, it is characterised in that：It is described
Step 2）In, the addition quality of the flocculant is 0.02-0.04% with the extracting solution mass ratio.
11. the method for vacuum and low temperature extraction folium sennae active ingredient according to claim 7, it is characterised in that：The step
Rapid 2）In, the ultrafiltration filter membrane uses cellulose acetate film, polyamide, polyether sulfone or hollow cellulose film.
12. the method for vacuum and low temperature extraction folium sennae active ingredient according to claim 7, it is characterised in that：The step
Rapid 4）In, the granularity of the mist particle is 200 mesh.
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| 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 |
| CN105254689B (en) * | 2015-11-04 | 2018-12-04 | 安徽九方药物研究院有限公司 | Sennoside AB salt compound and its preparation method and application |
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