CN102040637A - Method for extracting sennoside - Google Patents
Method for extracting sennoside Download PDFInfo
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- CN102040637A CN102040637A CN2010102931476A CN201010293147A CN102040637A CN 102040637 A CN102040637 A CN 102040637A CN 2010102931476 A CN2010102931476 A CN 2010102931476A CN 201010293147 A CN201010293147 A CN 201010293147A CN 102040637 A CN102040637 A CN 102040637A
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- anthraglucosennin
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Abstract
The invention relates to a method for extracting sennoside. The process method comprises the following steps of: crushing senna leaf, adding alkaline water in an amount which is 8 to 15 times that of the senna leaf, soaking and extracting for 2 to 3 times, regulating to reach neutrality, adding a precipitating agent for precipitating, and centrifuging; adding macroporous resin into extract for adsorbing, and eluting by using 40 to 70 percent ethanol solution; adding eluent into an ultrafiltration membrane system for ultrafiltration, collecting permeate, regulating the pH to be between 8 and 9, and concentrating by using a nanofiltration membrane; and regulating the pH of concentrated solution to be between 3 and 5, precipitating, filtering off a precipitate, dissolving in 80 to 95 percent ethanol saturated solution of which the pH is between 9 and 10, regulating to reach neutrality, standing for crystallizing, washing by using absolute ethanol, and drying in vacuum to obtain a product. The method is easy to operate, low in energy consumption, high in the yield and quality of the product, and suitable for industrial production.
Description
Technical field:
The invention belongs to biological technical field, especially relate to a kind of extracting method of anthraglucosennin.
Background technology:
Sennae is the leaflet of narrow leaf cassia angustifolia of leguminous plants or cassia acutifolia Delile, has the row that purges heat and stagnates, and defaecation, the Li Shui effect, the clinical digestive system that is used for the treatment of is as treatment constipation, intestinal obstruction.And the recovery of preoperative bowel lavage and postoperative intestinal function, taking on a small quantity can the defaecation fat-reducing.Be most popular in the world catharsis agent, safe in Western medicine, many countries are all opening the senna preparation of knowing clearly.
Anthraglucosennin is a sennae, is the main function composition, belongs to anthraquinone glycoside, mainly is Sennoside A, B.
Anthraglucosennin has under very strong the rushing down, but oral toxic side effect is very little, and anthraglucosennin is slowly to be hydrolyzed into aglycon through intestines bacterium enzyme, produces laxative action.
The light yellow crystalline powder of anthraglucosennin, water insoluble, ether, chloroform are slightly soluble in methyl alcohol, ethanol, acetone, are dissolved in alkaline aqueous solution.Sennoside A molecular weight: 739; Sennoside B molecular weight: 862.739.
The existing method of extracting anthraglucosennin mainly is classical anthraquinone class extractive crystallization process and column chromatography.
As patent " total sennoside extract of treatment constipation ", the method of this patent disclosure is to get the sennae medicinal material, add solvent, adopt reflux or insulation to soak and extract last macroporous adsorptive resins, water wash-out impurity, with low pure impurity elimination, the ethanolic soln wash-out is collected ethanol eluate again, concentrate eluant, drying get pale brown toner end extract then.
Extraction process organic solvent usage quantity is more, the residual bad control of reagent, and cost is higher, and the resin column method has very big advantage at enriching and purifying than extraction process, and cost is low, and because the easy oxygenolysis of anthraglucosennin, it is improper that concentration method is selected, and also can cause yield lower.
Summary of the invention:
The technical problem to be solved in the present invention provides the extracting method of a kind of yield height, anthraglucosennin that energy consumption is low.
For addressing the above problem, the present invention takes following technical scheme:
A kind of extracting method of anthraglucosennin is characterized in that comprising following steps:
1) extract: sennae is pulverized, add 6-15 and doubly measure alkaline water immersion extraction 2-3 time, regulate neutrality, with the sinking agent precipitation, the centrifugal extracting solution that gets;
2) macroporous resin adsorption: said extracted liquid adds macroporous resin adsorption, washes sugared reaction negative, and 40-70% ethanolic soln wash-out gets elutriant;
3) membrane sepn: the ultrafiltration of above-mentioned elutriant adding ultrafiltration membrane system, collect and see through liquid adjusting pH8-9, concentrate with nanofiltration membrane again, get concentrated solution;
4) crystallization: concentrated solution is regulated the pH3-5 precipitation, leach the 80-95% ethanol saturated dissolving of throw out with pH9-10, regulate the neutral crystallization of placing, absolute ethanol washing vacuum-drying promptly gets product.
Buck is yellow soda ash or the sodium hydrogen carbonate solution of 1-3% in the described step 1), and sinking agent is a CTS Chinese medicine finings, and consumption is the 0.5-2% of liquid.
Described step 2) a kind of among the optional HZ818 of macroporous resin model, LSA-33 in and the ADS-21, reverse upper prop, the eluent consumption is the 5-8BV of resin column.
The composite tube type film of the optional molecular weight cut-off 3000-20000 of ultra-filtration membrane in the described step 3), nanofiltration membrane are the composite tube type film of molecular weight cut-off 400-500, intake pressure 0.5-0.8mpa.
The acid of regulating pH in the described step is sulfuric acid or hydrochloric acid soln, and alkali is yellow soda ash or sodium hydrogen carbonate solution
Advantage of the present invention in sum is:
1) adopts the sinking agent precipitated impurities, can improve the resin absorption amount, prolong resin work-ing life.
2) to concentrate all be to carry out at normal temperatures for ultrafiltration membrance filter, nanofiltration membrane, avoided the loss of the anthraglucosennin in the high temperature concentration process, also cuts down the consumption of energy.
3) agents useful for same toxicological harmless of the present invention, superior product quality.
Embodiment:
Embodiment 1:
Sennae is pulverized, take by weighing 500g, put into little rust steel drum, adding 3% sodium hydrogen carbonate solution 5L soaked 3 hours, filter, the sodium bicarbonate that filter residue adds 4L3% soaks extraction 2 hours, filter, the sodium bicarbonate that filter residue adds 3L3% soaks extraction 1 hour, filter, merging filtrate, add 10% hydrochloric acid in the filtrate and be adjusted to neutrality, add the CTS Chinese medicine finings of 0.12L again, leave standstill, rotating speed with 20000r/s is centrifugal, the reverse upper prop of centrifugate is 60cm by the post height, and the LSA-33 type macroporous resin column of the 400g of post footpath 4cm is negative to be washed to the sugar reaction, use the ethanol liquid wash-out of 2.4L 50% again, the composite tube type film system that elutriant adds molecular weight cut-off 3000 carries out ultrafiltration, and intake pressure is controlled at 0.5-0.6mpa, sees through liquid and regulates pH9 with 3% sodium hydrogen carbonate solution again, the nanofiltration membrane of molecular weight cut-off 400 concentrates, intake pressure is 0.7-0.8mpa, concentrated solution, concentrated solution is adjusted to pH3-5 with 10% hydrochloric acid soln separates out precipitation, leach throw out 11g, with the saturated dissolving of 90% ethanol of pH9, regulate neutrality place crystallisate, with absolute ethanol washing crystallization 3 times, vacuum-drying promptly gets product 5.5g, content 98.3%.
Embodiment 2:
Sennae is pulverized, take by weighing 1Kg, put into stainless steel cask, adding 3% sodium carbonate solution 10L soaked 3 hours, filter, filter residue adds the soaking through sodium carbonate of 8L3% and extracted 2 hours, filter, filter residue adds the soaking through sodium carbonate of 6L3% and extracted 2 hours, filter, merging filtrate, add 10% sulfuric acid in the filtrate and be adjusted to neutrality, add the CTS Chinese medicine finings of 0.4L again, leave standstill, centrifugal, the reverse upper prop of centrifugate is the 800g ADS-21 type macroporous resin column of 50cm post footpath 6cm by the post height, negative to be washed to the sugar reaction, the ethanol liquid wash-out with 5.6L40% gets elutriant again, and the composite tube type film that elutriant adds molecular weight cut-off 10000 carries out ultrafiltration, intake pressure is controlled at 0.4-0.5mpa, see through liquid and regulate pH8 with 1% sodium carbonate solution, the nanofiltration membrane of molecular weight cut-off 500 concentrates, and intake pressure is 0.5-0.7mpa, get concentrated solution, concentrated solution is adjusted to pH5 with 5% sulphuric acid soln separates out precipitation, throw out 30g, with the saturated dissolving of 80% ethanol of pH9, regulate neutrality place crystallisate, with absolute ethanol washing crystallisate 3 times, vacuum-drying promptly gets product 13g, content 97.5%.
Embodiment 3:
Sennae is pulverized, take by weighing 1Kg, put into stainless steel cask, adding 1% sodium carbonate solution 15L soaked 5 hours, filter, filter residue adds the soaking through sodium carbonate of 15L1% and extracted 3 hours, merging filtrate, add 10% sulfuric acid in the filtrate and be adjusted to neutrality, the CTS Chinese medicine finings that adds 0.3L again, leave standstill, centrifugal, the reverse upper prop of centrifugate is the 700gHZ818 type macroporous resin column of 100cm post footpath 4cm by the post height, negative to be washed to the sugar reaction, ethanol liquid wash-out with 3.5L70% gets elutriant again, the composite tube type film that elutriant adds molecular weight cut-off 6000 carries out ultrafiltration, and intake pressure is controlled at 0.6-0.7mpa, sees through liquid and regulates pH8 with 1% sodium carbonate solution, the nanofiltration membrane of molecular weight cut-off 500 concentrates, intake pressure is 0.5-0.7mpa, concentrated solution, concentrated solution is adjusted to pH4 with 3% sulphuric acid soln separates out precipitation, get throw out 27g, with the saturated dissolving of 95% ethanol of pH8, regulate neutrality place crystallisate, with absolute ethanol washing crystallisate 2 times, vacuum-drying promptly gets product 11g, content 98%.
Embodiment 4:
Sennae is pulverized, take by weighing 1Kg, put into stainless steel cask, adding 1% sodium carbonate solution 10L soaked 3 hours, filter, filter residue adds the soaking through sodium carbonate of 8L1% and extracted 2 hours, filter, filter residue adds the soaking through sodium carbonate of 6L1% and extracted 2 hours, filter, merging filtrate, add 10% sulfuric acid in the filtrate and be adjusted to neutrality, add the CTS Chinese medicine finings of 0.5L again, leave standstill, centrifugal, the reverse upper prop of centrifugate is the 700g LSA-33 type macroporous resin column of 100cm post footpath 4cm by the post height, negative to be washed to the sugar reaction, the ethanol liquid wash-out with 5.6L50% gets elutriant again, and the composite tube type film that elutriant adds molecular weight cut-off 6000 carries out ultrafiltration, intake pressure is controlled at 0.5-0.6mpa, see through liquid and regulate pH9 with 1% sodium carbonate solution, the nanofiltration membrane of molecular weight cut-off 500 concentrates, and intake pressure is 0.5-0.7mpa, get concentrated solution, concentrated solution is adjusted to pH3 with 10% sulphuric acid soln separates out precipitation, get throw out 15g, with the saturated dissolving of 85% ethanol of pH9, regulate neutrality place crystallisate, with absolute ethanol washing crystallisate 3 times, vacuum-drying promptly gets product 10g, content 98.1%.
Embodiment 5:
Sennae is pulverized, take by weighing 2Kg, put into stainless steel cask, adding 1% sodium carbonate solution 20L soaked 3 hours, filter, filter residue adds the soaking through sodium carbonate of 15L1% and extracted 2 hours, filter, filter residue adds the soaking through sodium carbonate of 15L1% and extracted 2 hours, filter, merging filtrate, add 10% hydrochloric acid in the filtrate and be adjusted to neutrality, add the CTS Chinese medicine finings of 0.6L again, leave standstill, centrifugal, the reverse upper prop of centrifugate is the 1400gHZ818 type macroporous resin column of 100cm post footpath 6cm by the post height, negative to be washed to the sugar reaction, the ethanol liquid wash-out with 8L50% gets elutriant again, and the composite tube type film that elutriant adds molecular weight cut-off 10000 carries out ultrafiltration, intake pressure is controlled at 0.6-0.7mpa, see through liquid and regulate pH8 with 1% sodium carbonate solution, the nanofiltration membrane of molecular weight cut-off 500 concentrates, and intake pressure is 0.5-0.7mpa, get concentrated solution, concentrated solution is adjusted to pH4 with 5% hydrochloric acid soln separates out precipitation, throw out 32g, with the saturated dissolving of 90% ethanol of pH9, regulate neutrality place crystallisate, with outstanding water-ethanol wash crystallization thing 3 times, vacuum-drying promptly gets product 24g, content 98%.
Claims (5)
1. the extracting method of an anthraglucosennin is characterized in that comprising following steps:
1) extract: sennae is pulverized, add 6-15 and doubly measure alkaline water immersion extraction 2-3 time, regulate neutrality, with the sinking agent precipitation, the centrifugal extracting solution that gets;
2) macroporous resin adsorption: said extracted liquid adds macroporous resin adsorption, washes sugared reaction negative, and 40-70% ethanolic soln wash-out gets elutriant;
3) membrane sepn: the ultrafiltration of above-mentioned elutriant adding ultrafiltration membrane system, collect and see through liquid adjusting pH8-9, concentrate with nanofiltration membrane again, get concentrated solution;
4) crystallization: concentrated solution is regulated the pH3-5 precipitation, leach the 80-95% ethanol saturated dissolving of throw out with pH9-10, regulate the neutral crystallization of placing, absolute ethanol washing vacuum-drying promptly gets product.
2. the extracting method of anthraglucosennin according to claim 1 is characterized in that buck is yellow soda ash or the sodium hydrogen carbonate solution of 1-3% in the described step 1), and sinking agent is a CTS Chinese medicine finings, and consumption is the 0.5-2% of liquid.
3. the extracting method of anthraglucosennin according to claim 1 is characterized in that described step 2) in the optional HZ818 of macroporous resin model, LSA-33 and ADS-21 in a kind of, reverse upper prop, the eluent consumption is the 5-8BV of resin column.
4. the extracting method of anthraglucosennin according to claim 1 is characterized in that the composite tube type film of the optional molecular weight cut-off 3000-20000 of ultra-filtration membrane in the described step 3), and nanofiltration membrane is the composite tube type film of molecular weight cut-off 400-500, intake pressure 0.5-0.8mpa.
5. the extracting method of anthraglucosennin according to claim 1, the acid that it is characterized in that regulating in the described step pH is sulfuric acid or hydrochloric acid soln, alkali is yellow soda ash or sodium hydrogen carbonate solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102931476A CN102040637A (en) | 2010-09-27 | 2010-09-27 | Method for extracting sennoside |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010102931476A CN102040637A (en) | 2010-09-27 | 2010-09-27 | Method for extracting sennoside |
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| CN102040637A true CN102040637A (en) | 2011-05-04 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105254689A (en) * | 2015-11-04 | 2016-01-20 | 安徽九方药物研究院有限公司 | Sennoside A.B salt compound as well as preparation method and application thereof |
| CN106478748A (en) * | 2016-08-31 | 2017-03-08 | 重庆方通动物药业有限公司 | The method that vacuum and low temperature extracts Folium Sennae effective ingredient |
| CN109966337A (en) * | 2019-03-28 | 2019-07-05 | 湖南华诚生物资源股份有限公司 | A method of extracting sennoside from folium sennae |
| CN112353835A (en) * | 2020-10-29 | 2021-02-12 | 宁波绿之健药业有限公司 | Water-soluble senna leaf extract, preparation process and application |
| CN113861250A (en) * | 2021-11-11 | 2021-12-31 | 江苏艾迪药业股份有限公司 | A method for preparing high purity sennoside and sennoside or its derivatives |
| CN114031654A (en) * | 2021-11-11 | 2022-02-11 | 江苏艾迪药业股份有限公司 | Sennoside extraction method |
-
2010
- 2010-09-27 CN CN2010102931476A patent/CN102040637A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105254689A (en) * | 2015-11-04 | 2016-01-20 | 安徽九方药物研究院有限公司 | Sennoside A.B salt compound as well as preparation method and application thereof |
| 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 |
| CN106478748A (en) * | 2016-08-31 | 2017-03-08 | 重庆方通动物药业有限公司 | The method that vacuum and low temperature extracts Folium Sennae effective ingredient |
| CN109966337A (en) * | 2019-03-28 | 2019-07-05 | 湖南华诚生物资源股份有限公司 | A method of extracting sennoside from folium sennae |
| CN112353835A (en) * | 2020-10-29 | 2021-02-12 | 宁波绿之健药业有限公司 | Water-soluble senna leaf extract, preparation process and application |
| CN113861250A (en) * | 2021-11-11 | 2021-12-31 | 江苏艾迪药业股份有限公司 | A method for preparing high purity sennoside and sennoside or its derivatives |
| CN114031654A (en) * | 2021-11-11 | 2022-02-11 | 江苏艾迪药业股份有限公司 | Sennoside extraction method |
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Application publication date: 20110504 |