CN1699403A - Process for extracting sarsasapogenin from Chinese traditional medicines - Google Patents
Process for extracting sarsasapogenin from Chinese traditional medicines Download PDFInfo
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- CN1699403A CN1699403A CN 200510049813 CN200510049813A CN1699403A CN 1699403 A CN1699403 A CN 1699403A CN 200510049813 CN200510049813 CN 200510049813 CN 200510049813 A CN200510049813 A CN 200510049813A CN 1699403 A CN1699403 A CN 1699403A
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- smilagenin
- chinese medicinal
- medicinal materials
- extracting
- solution
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- RTMWIZOXNKJHRE-UHFFFAOYSA-N Tigogenin Natural products CC1COC2CC(C)(OC12)C3CCC4C5CCC6CC(O)CCC6(C)C5CCC34C RTMWIZOXNKJHRE-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 21
- GMBQZIIUCVWOCD-WWASVFFGSA-N Sarsapogenine Chemical compound O([C@@H]1[C@@H]([C@]2(CC[C@@H]3[C@@]4(C)CC[C@H](O)C[C@H]4CC[C@H]3[C@@H]2C1)C)[C@@H]1C)[C@]11CC[C@H](C)CO1 GMBQZIIUCVWOCD-WWASVFFGSA-N 0.000 title abstract 4
- 229940126672 traditional medicines Drugs 0.000 title abstract 2
- 238000002386 leaching Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000002425 crystallisation Methods 0.000 claims abstract description 5
- 230000008025 crystallization Effects 0.000 claims abstract description 5
- 239000011347 resin Substances 0.000 claims abstract description 5
- 229920005989 resin Polymers 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- GMBQZIIUCVWOCD-UQHLGXRBSA-N (25R)-5beta-spirostan-3beta-ol Chemical compound O([C@@H]1[C@@H]([C@]2(CC[C@@H]3[C@@]4(C)CC[C@H](O)C[C@H]4CC[C@H]3[C@@H]2C1)C)[C@@H]1C)[C@]11CC[C@@H](C)CO1 GMBQZIIUCVWOCD-UQHLGXRBSA-N 0.000 claims description 62
- 229950002323 smilagenin Drugs 0.000 claims description 31
- 239000000463 material Substances 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- 230000001476 alcoholic effect Effects 0.000 claims description 18
- 238000000967 suction filtration Methods 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 9
- 241000432824 Asparagus densiflorus Species 0.000 claims description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 241000234280 Liliaceae Species 0.000 claims description 5
- 238000010828 elution Methods 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 238000000926 separation method Methods 0.000 abstract description 3
- 238000005903 acid hydrolysis reaction Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 32
- 239000000284 extract Substances 0.000 description 5
- 239000003814 drug Substances 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 238000004061 bleaching Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 241000411851 herbal medicine Species 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 230000035922 thirst Effects 0.000 description 2
- 208000024827 Alzheimer disease Diseases 0.000 description 1
- 241000605445 Anemarrhena asphodeloides Species 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- 206010013954 Dysphoria Diseases 0.000 description 1
- 208000015220 Febrile disease Diseases 0.000 description 1
- 206010034719 Personality change Diseases 0.000 description 1
- 208000001431 Psychomotor Agitation Diseases 0.000 description 1
- 206010038743 Restlessness Diseases 0.000 description 1
- 206010039966 Senile dementia Diseases 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229940088623 biologically active substance Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 208000021760 high fever Diseases 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- 230000002218 hypoglycaemic effect Effects 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000035807 sensation Effects 0.000 description 1
- 208000010110 spontaneous platelet aggregation Diseases 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 201000008827 tuberculosis Diseases 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a process for extracting sarsasapogenin from Chinese traditional medicines by means of macroporous resin separation and crystallization technique, which comprises the steps of drying and disintegrating the raw material, leaching, concentrating under reduced pressure, gradient eluting, acid hydrolysis, decolorizing and crystallizing.
Description
Technical field
The present invention relates to the separation purification method of biologically active substance in a kind of biotechnology, particularly utilize the method for macroporous resin separation and crystallization technique batch extracting Smilagenin from Chinese medicinal materials.
Background technology
Smilagenin is a kind of white needle, extensively be present in the Liliaceae herbal medicine such as the wind-weed, asparagus fern, have crucial physiological action, have clearing heat and detoxicating, the relieving restlessness of quenching the thirst, the moistening lung nourshing kidney, antiviral, platelet aggregation-against, hypoglycemic, remove effects such as free radical, dysphoria with smothery sensation be can be used for curing mainly in the modern medicine and febrile disease high fever, cough due to lung-heat quenched one's thirst, the tuberculosis heating, diabetes are hard and dry, (the study of senile dementia and Aging, hypomnesis, or some personality change) etc. symptom.Therefore the potential a kind of necessary goods and materials that are widely used in medicine, food and cosmetic industry that become of Smilagenin have vast market prospect.
With Liliaceae Chinese medicinal materialss such as the wind-weed and asparagus fern be that the raw material production Smilagenin has that technology is simple, characteristics such as relative low production cost, raw material resources are abundant, so research and development extraction Smilagenin from Chinese medicinal materials has tangible economic worth and realistic meaning.But present extracting method all can only be realized a small amount of extraction, and the Smilagenin purity of extraction can not reach medicinal requirements, and the cost height also is not suitable for large-scale commercial production.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, a kind of method of batch extracting Smilagenin from Chinese medicinal materials of simple and effective is provided.
In order to solve the problems of the technologies described above, the present invention is achieved by the following technical solutions:
The invention provides a kind of method of from Chinese medicinal materials, extracting Smilagenin, may further comprise the steps:
(1) choose the Chinese medicinal materials that contains Smilagenin, crushed after being dried makes raw material powder particle diameter order number be not less than 200 orders:
(2) use alcoholic solution 20～70 ℃ of following lixiviate raw material powders 4～6 hours, raw material powder and alcoholic solution mass ratio are 1: 10～20, and alcoholic solution concentration is greater than 75% (V/V);
(3) separate first vat liquor, residue adds 5～10 times of alcoholic solutions and soaked once more under 20～70 ℃ 4～6 hours;
(4) merge twice vat liquor, be not higher than concentrating under reduced pressure under 70 ℃ of conditions;
(5) with sample on the spissated vat liquor to D101 macroporous resin pillar, carry out gradient elution with 1～3 times of column volume ethanolic soln, substep is collected elute soln;
(6) the gained elutriant is concentrated into 1/10 volume in the time of will be with 90% aqueous ethanolic solution wash-out, adds isopyknic 2% hydrochloric acid soln, acidolysis suction filtration after 2 hours under 50 ℃ of conditions;
(7) filter residue is dissolved in the anhydrous ethanol solvent, adds proper amount of active carbon, decoloured 30 minutes down in 45～60 ℃, suction filtration is removed gac impurity.
(8) concentrated filtrate make 50 ℃ down to degree of saturation and crystallization under room temperature, suction filtration goes out needle crystal, is drying to obtain the Smilagenin product.
Leaching alcohol solution of the present invention is ethanolic soln.
Leaching alcohol solution of the present invention is butanol solution.
Leaching alcohol strength of solution of the present invention is 95% (V/V).
Wash-out alcoholic solution of the present invention is an ethanolic soln.
Crystal alcohol solution of the present invention is anhydrous ethanol solvent.
The Chinese medicinal materials that contains Smilagenin of the present invention is Liliaceae Chinese medicinal materialss such as the wind-weed and asparagus fern.
Compared with prior art, the invention has the beneficial effects as follows:
Use product that the method for the invention obtains needle-like crystal as white, the crystal shape rule, the melting range scope is short.Because the recrystallisation solvent that uses is an ethanol, the products obtained therefrom reliable in quality does not have any murder by poisoning organic solvent residual.Product can be used as the synthesis material of hormone drugs in the medicine industry, also can be used as the Smilagenin standard substance and uses.
Embodiment
Below the present invention is further described by specific embodiment.
Raw material of the present invention can be chosen the Chinese medicinal materials that contains Smilagenin, such as the wind-weed, and Liliaceae herbal medicine such as asparagus fern.
Specific embodiment 1:
From the Chinese medicinal materials wind-weed, extract the method for Smilagenin, may further comprise the steps:
Get the 10kg exsiccant wind-weed (not boiling is directly dried) and be cut into segment with chopper, then the segment that is cut into is pulverized with pulverizer, its order number is not less than 200 orders, if once pulverize inadequately, can repeatedly pulverize;
The edible ethanol that adds 200 liter 95% in above-mentioned 10kg Common Anemarrhena Rhizome is refunded in the lixiviate jar after with wooden stick its suspension liquid being stirred evenly, and lixiviate is 6 hours under 70 ℃ of conditions.Stir in the leaching process, realize that dynamic constant temperature extracts;
Above-mentioned suspension is placed the suction filter suction filtration, add 100 liter of 90% edible ethanol then in suction filtration is residue obtained, continued under 70 ℃ of conditions dynamic extraction 6 hours, suction filtration in suction filter discards residue then.
Collect the filtrate behind the suction filtration twice, join in the triple effect alcohol distillation column, reclaim under reduced pressure alcohol, up to solution be original volume 1/10 till, the alcohol rate of recovery is generally about 80%.Solution after concentrating is joined in the Rotary Evaporators for 30 liters in batches, and decompression fully concentrates under 50 ℃ of conditions, directly goes up sample to the D101 macroporous resin pillar that pre-treatment is good for 10 liters with concentrating good extracting solution at last.
Aqueous ethanolic solution with 3 times of column volume 10%, 30%, 50%, 90% different ratioss carries out wash-out respectively.The elutriant of gained places Rotary Evaporators for 15 liters in the time of will be with 90% aqueous ethanolic solution wash-out, is concentrated to 2 liters under 50 ℃ of conditions.
In above-mentioned 2 liters of concentrated solutions, add the hydrochloric acid soln of equal-volume 2%, place 50 ℃ of following acidolysis about 2 hours.With the acid hydrolysis solution suction filtration, filtering filter residue dissolves with anhydrous ethanol solvent after the acidolysis.Add in above-mentioned crystal alcohol solution 200ml about gac 4 spoonfuls (20g), in 50 ℃ of decolourings 30 minutes down, suction filtration falls the gac part then.
Be adjusted to state of saturation under 50 ℃ of the filtrate 200ml solution that suction filtration is gone out, solution is placed crystallization under the room temperature.Suction filtration goes out the white needle-like crystals of analysing in batches, places vacuum drier, and drying under reduced pressure obtains Smilagenin sample 46g.
Specific embodiment 2:
The operation steps of extracting is identical with embodiment 1, wherein:
The alcoholic solution of lixiviate is that concentration is the propyl carbinol of 75% (V/V), and raw material powder and alcoholic solution mass ratio are 1: 10,20 ℃ of leaching temperatures, and the time is 4 hours.Leaching back concentrating under reduced pressure temperature is 70 ℃, and bleaching temperature is 45 ℃, and the usage quantity of the alcoholic solution during gradient elution is 2 times of column volumes, obtains Smilagenin sample 44.7g.
Specific embodiment 3:
From the Chinese medicinal materials asparagus fern, extract the method for Smilagenin, may further comprise the steps:
Get 10kg exsiccant asparagus fern (not boiling is directly dried) and be cut into segment with chopper, then the segment that is cut into is pulverized with pulverizer, its order number is not less than 200 orders, if once pulverize inadequately, can repeatedly pulverize; The operation steps of extracting is identical with embodiment 1, wherein:
The alcoholic solution of lixiviate is that concentration is the aqueous ethanolic solution of 95% (V/V), and raw material powder and alcoholic solution mass ratio are 1: 15,60 ℃ of leaching temperatures, and the time is 5 hours.Leaching back concentrating under reduced pressure temperature is 60 ℃, and bleaching temperature is 60 ℃, and the usage quantity of the alcoholic solution during gradient elution is 3 times of column volumes, obtains Smilagenin sample 28.3g.
Specific embodiment 4:
From the Chinese medicinal materials asparagus fern, extract the method for Smilagenin, may further comprise the steps:
The operation steps of extracting is identical with embodiment 1, wherein:
The alcoholic solution of lixiviate is that concentration is the n-butanol aqueous solution of 90% (V/V), and raw material powder and alcoholic solution mass ratio are 1: 15,50 ℃ of leaching temperatures, and the time is 6 hours.Leaching back concentrating under reduced pressure temperature is 60 ℃, and bleaching temperature is 60 ℃, and the usage quantity of the alcoholic solution during gradient elution is 1 times of column volume, obtains Smilagenin sample 27g.
At last, it is also to be noted that what more than enumerate only is specific embodiments of the invention.Obviously, the invention is not restricted to above examples of implementation, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (6)
1, a kind of method of extracting Smilagenin from Chinese medicinal materials is characterized in that may further comprise the steps:
(1) choose the Chinese medicinal materials that contains Smilagenin, crushed after being dried makes raw material powder particle diameter order number be not less than 200 orders;
(2) use alcoholic solution 20～70 ℃ of following lixiviate raw material powders 4～6 hours, raw material powder and alcoholic solution mass ratio are 1: 10～20, and alcoholic solution concentration is greater than 75% (V/V);
(3) separate first vat liquor, residue adds 5～10 times of alcoholic solutions and soaked once more under 20～70 ℃ 4～6 hours;
(4) merge twice vat liquor, be not higher than concentrating under reduced pressure under 70 ℃ of conditions;
(5) with sample on the spissated vat liquor to D101 macroporous resin pillar, carry out gradient elution with 1～3 times of column volume ethanolic soln, substep is collected elute soln;
The gained elutriant is concentrated into 1/10 volume during (6) with 90% aqueous ethanolic solution wash-out, adds isopyknic 2% hydrochloric acid soln, acidolysis suction filtration after 2 hours under 50 ℃ of conditions;
(7) filter residue is dissolved in the anhydrous ethanol solvent, adds proper amount of active carbon, decoloured 30 minutes down in 45～60 ℃, suction filtration is removed gac impurity.
(8) concentrated filtrate make 50 ℃ down to degree of saturation and crystallization under room temperature, suction filtration goes out needle crystal, is drying to obtain the Smilagenin product.
2, the method for extracting Smilagenin from Chinese medicinal materials according to claim 1 is characterized in that described leaching alcohol solution is ethanolic soln.
3, the method for extracting Smilagenin from Chinese medicinal materials according to claim 1 is characterized in that described leaching alcohol solution is butanol solution.
4, the method for extracting Smilagenin from Chinese medicinal materials according to claim 1 is characterized in that described leaching alcohol strength of solution is 95% (V/V).
5, the method for extracting Smilagenin from Chinese medicinal materials according to claim 1 is characterized in that the described Chinese medicinal materials that contains Smilagenin is the wind-weed.
6, the method for extracting Smilagenin from Chinese medicinal materials according to claim 1 is characterized in that the described Chinese medicinal materials that contains Smilagenin is asparagus fern or other Liliaceae Chinese medicinal materials.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100498130A CN100335493C (en) | 2005-05-24 | 2005-05-24 | Process for extracting sarsasapogenin from Chinese traditional medicines |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100498130A CN100335493C (en) | 2005-05-24 | 2005-05-24 | Process for extracting sarsasapogenin from Chinese traditional medicines |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1699403A true CN1699403A (en) | 2005-11-23 |
| CN100335493C CN100335493C (en) | 2007-09-05 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100498130A Expired - Fee Related CN100335493C (en) | 2005-05-24 | 2005-05-24 | Process for extracting sarsasapogenin from Chinese traditional medicines |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768202A (en) * | 2009-02-18 | 2010-07-07 | 沈阳药科大学 | Preparing method of high purity sarsasapogenin in rhizoma anemarrhenae and derivatives thereof, and medical new application thereof |
| CN101401896B (en) * | 2008-09-28 | 2011-06-22 | 湖北福人药业股份有限公司 | Extracting method of active principle of sarsaparilla |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1203083C (en) * | 2003-02-25 | 2005-05-25 | 广州莱泰制药有限公司 | Rhizoma anemarrhenae extract and preparation process and use thereof |
| CN1199643C (en) * | 2003-05-09 | 2005-05-04 | 中国人民解放军第二军医大学 | Use of timosaponin for preparing medicine for preventing and treating brain apoplexy |
-
2005
- 2005-05-24 CN CNB2005100498130A patent/CN100335493C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101401896B (en) * | 2008-09-28 | 2011-06-22 | 湖北福人药业股份有限公司 | Extracting method of active principle of sarsaparilla |
| CN101768202A (en) * | 2009-02-18 | 2010-07-07 | 沈阳药科大学 | Preparing method of high purity sarsasapogenin in rhizoma anemarrhenae and derivatives thereof, and medical new application thereof |
| CN101768202B (en) * | 2009-02-18 | 2013-10-30 | 沈阳药科大学 | Preparing method of high purity sarsasapogenin in rhizoma anemarrhenae and derivatives thereof, and medical new application thereof |
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| Publication number | Publication date |
|---|---|
| CN100335493C (en) | 2007-09-05 |
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Granted publication date: 20070905 Termination date: 20130524 |