CN102327316A - Method for extracting total saponins from fructus gleditsiae - Google Patents
Method for extracting total saponins from fructus gleditsiae Download PDFInfo
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- CN102327316A CN102327316A CN201110187514A CN201110187514A CN102327316A CN 102327316 A CN102327316 A CN 102327316A CN 201110187514 A CN201110187514 A CN 201110187514A CN 201110187514 A CN201110187514 A CN 201110187514A CN 102327316 A CN102327316 A CN 102327316A
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- fructus gleditsiae
- total saponins
- gleditsiae abnormalis
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Abstract
The invention relates to a method for extracting total saponins from fructus gleditsiae, which comprises the following steps of: firstly, crushing fructus gleditsiae dried medicinal material, adding 5-8 volumes by weight of lower alcohol water solution, carrying out ultrasound extraction for 2-3 times and filtering to obtain an extraction solution; secondly, carrying out condensation under reduced pressure on the extraction solution until no alcohol flavor exists, adding the extraction solution in a macroporous resin column, washing with water or 10-20 percent ethanol solution to remove impurities, eluting with 55-70 percent of ethanol solution and collecting an eluent; and thirdly, reducing the pressure and recovering the ethanol from the eluent, filtering through an ultrafiltration membrane, condensing filtrate through a nanofiltration membrane and drying to obtain the total saponins from the fructus gleditsiae. The method has the advantages of less pollution, low cost and high yield; and the obtained product has no solvent residue and can be directly used for producing foods and medicines.
Description
Technical field
The present invention relates to a kind of method of from Fructus Gleditsiae Abnormalis, extracting total saponins, particularly relate to a kind of method of utilizing column chromatography and membrane separation technique to extract the Fructus Gleditsiae Abnormalis total saponins.
Background technology
Fructus Gleditsiae Abnormalis is the dry sterile fruit of pulse family Caesalpinoidea Gleditsia plant Fructus Gleditsia.Fructus Gleditsia is the endemic species that distribute in China, and the distribution and cultivation area of coverage accounts for 50% of area.Fructus Gleditsia can form two kinds of fruits under different developmental conditions, ripe loose person is a Chinese honey locust (fruit), and ateliosis slight of stature person is a Fructus Gleditsiae Abnormalis." record be conventional Chinese medicine one of by 2005 editions by Chinese pharmacopoeia for Fructus Gleditsiae Abnormalis.Fructus Gleditsiae Abnormalis have eliminate the phlegm have one's ideas straightened out, the effect of dispersing swelling and dissipating binds, be mainly used in the apoplexy locked mouth, remain unconscious, the epilepsy abundant expectoration, close that key is obstructed, disease such as sore throat stagnation of phlegm, pertinacious phlegm are breathed with cough, expectoration is not well, constipation due to dry stool, external treatment are too fat to move.
Modern study finds that Fructus Gleditsiae Abnormalis mainly contains multiple triterpene saponin, has antiinflammatory, antiallergic, antitumor, antiviral, improves effect such as myocardial ischemia, and its antiinflammatory and active anticancer are more remarkable.
The existing Fructus Gleditsiae Abnormalis total saponins that extracts has extraction and column chromatography.Like patent (publication number CN1429834A) " Fructus Gleditsiae Abnormalis total saponins and preparation method thereof and its application in the preparation medicine ", this patent disclosed method is to adopt macroporous resin column chromatography and organic solvent extraction to obtain the Fructus Gleditsiae Abnormalis total saponins.Said method with an organic solvent extracts, and is unfavorable for environmental protection, and sample loss is big simultaneously.
Summary of the invention
The purpose of this invention is to provide a kind of method of from Fructus Gleditsiae Abnormalis, extracting total saponins.The present invention utilizes film to divide and column chromatography technology combines, and has not only improved and has extracted the yield of Fructus Gleditsiae Abnormalis total saponins, and can obtain high-quality Fructus Gleditsiae Abnormalis total saponins, and this method economy is simple simultaneously.
The present invention realizes through following technical scheme:
A kind of method of from Fructus Gleditsiae Abnormalis, extracting total saponins is characterized in that may further comprise the steps:
(1) supersound extraction: with the dry pulverizing medicinal materials of Fructus Gleditsiae Abnormalis, add 5-8 and doubly measure low carbon alcohol solution, supersound extraction 2-3 time is filtered and is obtained extracting solution;
(2) column chromatography: extracting solution is evaporated to does not have the alcohol flavor, adds macroporous resin column, the alcoholic solution flush away impurity of first water or 10-20%, and the alcoholic solution eluting of reuse 55-70% is collected eluent;
(3) membrance separation: the eluent decompression recycling ethanol, filter through ultrafilter membrane, filtrating concentrates through NF membrane again, and lyophilization promptly gets the Fructus Gleditsiae Abnormalis total saponins.
Said low carbon alcohol solution is the 45-75% ethanol water, and the supersound extraction frequency is 25-50KHz.
Said macroporous resin is HP20, HPD300, XAD-16 or XSD-3 type, and the consumption of macroporous resin is 0.5-1 a times of medical material weight.
Said ultrafilter membrane is the hollow fiber ultrafiltration film of molecular cut off 5000-10000, and NF membrane is that molecular cut off is 1000 hollow NF membrane.
The invention has the beneficial effects as follows:
(1) organic residual low.The present invention has abandoned solvent extraction technology in the traditional handicraft, and final products employing lyophilization processing, so the organic solvent residual of final products is especially little.
(2) cycle is short.The present invention adopts column chromatography and membrane separation technique to combine, and has improved separation efficiency greatly.
(3) the sample yield is high.Adopt the method for membrance separation to carry out remove impurity in the leaching process and concentrate, avoided the incomplete shortcoming of solvent extraction in the traditional handicraft, sample loss is few simultaneously.
(4) the inventive method is simple, is easy to grasp, and efficient is high.
The specific embodiment
To combine the specific embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment 1
With the dry pulverizing medicinal materials of Fructus Gleditsiae Abnormalis, get 1kg, add 8 times of amount 60% ethanol waters, supersound extraction 2 times; The extraction frequency is 30KHz, filters and obtains extracting solution, and being evaporated to does not have the alcohol flavor; Add HPD300 type macroporous resin column, the consumption of macroporous resin is 1kg, first water flush away impurity; The alcoholic solution eluting of reuse 55% is collected eluent, decompression recycling ethanol; Through the hollow fiber ultrafiltration membrane filtration mistake of molecular cut off 5000-10000, filtrating is that 1000 hollow NF membrane concentrates through molecular cut off again, and lyophilization promptly gets Fructus Gleditsiae Abnormalis total saponins 142g.
Embodiment 2
With the dry pulverizing medicinal materials of Fructus Gleditsiae Abnormalis, get 1kg, add 6 times of amount 75% ethanol waters, supersound extraction 2 times; The extraction frequency is 25KHz, filters and obtains extracting solution, and being evaporated to does not have the alcohol flavor; Add XAD-16 type macroporous resin column, the consumption of macroporous resin is 500g, earlier with 20% alcoholic solution flush away impurity; The alcoholic solution eluting of reuse 60% is collected eluent, decompression recycling ethanol; Through the hollow fiber ultrafiltration membrane filtration mistake of molecular cut off 5000-10000, filtrating is that 1000 hollow NF membrane concentrates through molecular cut off again, and lyophilization promptly gets Fructus Gleditsiae Abnormalis total saponins 125g.
Embodiment 3
With the dry pulverizing medicinal materials of Fructus Gleditsiae Abnormalis, get 3kg, add 5 times of amount 45% ethanol waters, supersound extraction 3 times; The extraction frequency is 50KHz, filters and obtains extracting solution, and being evaporated to does not have the alcohol flavor; Add HP20 type macroporous resin column, the consumption of macroporous resin is 1.5kg, first water flush away impurity; The alcoholic solution eluting of reuse 55% is collected eluent, decompression recycling ethanol; Through the hollow fiber ultrafiltration membrane filtration mistake of molecular cut off 5000-10000, filtrating is that 1000 hollow NF membrane concentrates through molecular cut off again, and lyophilization promptly gets Fructus Gleditsiae Abnormalis total saponins 440g.
Embodiment 4
With the dry pulverizing medicinal materials of Fructus Gleditsiae Abnormalis, get 3kg, add 6 times of amount 65% ethanol waters, supersound extraction 3 times; The extraction frequency is 45KHz, filters and obtains extracting solution, and being evaporated to does not have the alcohol flavor; Add XSD-3 type macroporous resin column, the consumption of macroporous resin is 2kg, first water flush away impurity; The alcoholic solution eluting of reuse 60% is collected eluent, decompression recycling ethanol; Through the hollow fiber ultrafiltration membrane filtration mistake of molecular cut off 5000-10000, filtrating is that 1000 hollow NF membrane concentrates through molecular cut off again, and lyophilization promptly gets Fructus Gleditsiae Abnormalis total saponins 405g.
Embodiment 5
With the dry pulverizing medicinal materials of Fructus Gleditsiae Abnormalis, get 5kg, add 8 times of amount 60% ethanol waters, supersound extraction 3 times; The extraction frequency is 40KHz, filters and obtains extracting solution, and being evaporated to does not have the alcohol flavor; Add XAD-16 type macroporous resin column, the consumption of macroporous resin is 5kg, earlier with 10% alcoholic solution flush away impurity; The alcoholic solution eluting of reuse 55% is collected eluent, decompression recycling ethanol; Through the hollow fiber ultrafiltration membrane filtration mistake of molecular cut off 5000-10000, filtrating is that 1000 hollow NF membrane concentrates through molecular cut off again, and lyophilization promptly gets Fructus Gleditsiae Abnormalis total saponins 751g.
Claims (4)
1. method of from Fructus Gleditsiae Abnormalis, extracting total saponins is characterized in that may further comprise the steps:
(1) supersound extraction: with the dry pulverizing medicinal materials of Fructus Gleditsiae Abnormalis, add 5-8 and doubly measure low carbon alcohol solution, supersound extraction 2-3 time is filtered and is obtained extracting solution;
(2) column chromatography: extracting solution is evaporated to does not have the alcohol flavor, adds macroporous resin column, the alcoholic solution flush away impurity of first water or 10-20%, and the alcoholic solution eluting of reuse 55-70% is collected eluent;
(3) membrance separation: the eluent decompression recycling ethanol, filter through ultrafilter membrane, filtrating concentrates through NF membrane again, is drying to obtain the Fructus Gleditsiae Abnormalis total saponins.
2. a kind of method of from Fructus Gleditsiae Abnormalis, extracting total saponins according to claim 1 is characterized in that low carbon alcohol solution is the 45-75% ethanol water described in the step (1), and the supersound extraction frequency is 25-50KHz.
3. a kind of method of from Fructus Gleditsiae Abnormalis, extracting total saponins according to claim 1 is characterized in that macroporous resin described in the step (2) is HP20, HPD300, XAD-16 or XSD-3 type, and the consumption of macroporous resin is 0.5-1 a times of medical material weight.
4. a kind of method of from Fructus Gleditsiae Abnormalis, extracting total saponins according to claim 1 is characterized in that ultrafilter membrane described in the step (3) is the hollow fiber ultrafiltration film of molecular cut off 5000-10000, and NF membrane is that molecular cut off is 1000 hollow NF membrane.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110187514A CN102327316A (en) | 2011-07-06 | 2011-07-06 | Method for extracting total saponins from fructus gleditsiae |
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| CN201110187514A CN102327316A (en) | 2011-07-06 | 2011-07-06 | Method for extracting total saponins from fructus gleditsiae |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103083388A (en) * | 2012-12-31 | 2013-05-08 | 山东省中医药研究院 | Preparation method of fructus gleditsiae total saponins |
| RU2510278C1 (en) * | 2012-08-08 | 2014-03-27 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Тверской государственный университет" | Method for preparing saponin-containing extracts (versions) |
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2011
- 2011-07-06 CN CN201110187514A patent/CN102327316A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2510278C1 (en) * | 2012-08-08 | 2014-03-27 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Тверской государственный университет" | Method for preparing saponin-containing extracts (versions) |
| CN103083388A (en) * | 2012-12-31 | 2013-05-08 | 山东省中医药研究院 | Preparation method of fructus gleditsiae total saponins |
| CN103083388B (en) * | 2012-12-31 | 2015-07-01 | 山东省中医药研究院 | Preparation method of fructus gleditsiae total saponins |
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Application publication date: 20120125 |