CN1111250A - Method for extracting diosgenin from Dioscorea plant - Google Patents
Method for extracting diosgenin from Dioscorea plant Download PDFInfo
- Publication number
- CN1111250A CN1111250A CN 94104778 CN94104778A CN1111250A CN 1111250 A CN1111250 A CN 1111250A CN 94104778 CN94104778 CN 94104778 CN 94104778 A CN94104778 A CN 94104778A CN 1111250 A CN1111250 A CN 1111250A
- Authority
- CN
- China
- Prior art keywords
- diosgenin
- extracting
- extraction
- yam
- ethanol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- DWCSNWXARWMZTG-UHFFFAOYSA-N Trigonegenin A Natural products CC1C(C2(CCC3C4(C)CCC(O)C=C4CCC3C2C2)C)C2OC11CCC(C)CO1 DWCSNWXARWMZTG-UHFFFAOYSA-N 0.000 title claims abstract description 28
- WQLVFSAGQJTQCK-VKROHFNGSA-N diosgenin Chemical compound O([C@@H]1[C@@H]([C@]2(CC[C@@H]3[C@@]4(C)CC[C@H](O)CC4=CC[C@H]3[C@@H]2C1)C)[C@@H]1C)[C@]11CC[C@@H](C)CO1 WQLVFSAGQJTQCK-VKROHFNGSA-N 0.000 title claims abstract description 28
- WQLVFSAGQJTQCK-UHFFFAOYSA-N diosgenin Natural products CC1C(C2(CCC3C4(C)CCC(O)CC4=CCC3C2C2)C)C2OC11CCC(C)CO1 WQLVFSAGQJTQCK-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 11
- 241000234273 Dioscorea Species 0.000 title abstract 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000000605 extraction Methods 0.000 claims abstract description 13
- 239000000284 extract Substances 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims 1
- 238000010992 reflux Methods 0.000 abstract description 5
- 238000010438 heat treatment Methods 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 244000281702 Dioscorea villosa Species 0.000 description 7
- 235000004879 dioscorea Nutrition 0.000 description 6
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 5
- 235000011116 calcium hydroxide Nutrition 0.000 description 5
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 5
- 229930182490 saponin Natural products 0.000 description 5
- 150000007949 saponins Chemical class 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000000920 calcium hydroxide Substances 0.000 description 4
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 2
- 230000001476 alcoholic effect Effects 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 235000005903 Dioscorea Nutrition 0.000 description 1
- 240000001811 Dioscorea oppositifolia Species 0.000 description 1
- 235000000504 Dioscorea villosa Nutrition 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 244000061458 Solanum melongena Species 0.000 description 1
- 235000002597 Solanum melongena Nutrition 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229930002875 chlorophyll Natural products 0.000 description 1
- 235000019804 chlorophyll Nutrition 0.000 description 1
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000003270 steroid hormone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Steroid Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for extracting diosgenin from dioscorea plants, which adopts ethanol as an extraction solvent and directly extracts diosgenin from the dioscorea plants by reflux heating.
Description
The present invention relates to a kind of method of from yam, extracting diosgenin.
Diosgenin (Diosogenin) claims diosgenin again, and chemical name is △, 3-hydroxyl, 25R-spirostene.It is the synthesizing steroid hormone medicine.Diosgenin can extract acquisition from yam.The existing diosgenin that extracts from yam all uses industrial naptha as extraction agent, and its method is to carry out to be incubated continuous extractive static state operation method in circulation extraction equipment.The efficient of extracting diosgenin in this way is low, and the time long (needing more than 10 hours) and the extraction yield of diosgenin only are 80-90%, still has 10% saponin to be stranded in the recrement.Simultaneously, industrial naptha is inflammable and explosive organic solvent, and safety easily has an accident inadequately.In addition, impurity such as by product △-Tigogenin when often containing hydrolysis in the saponin product with gasoline extraction and wax, this has influenced the quality of product.
The present invention is intended to propose a kind of extraction diosgenin method safe, high extraction.
The method of the extraction diosgenin that the present invention proposes is to adopt ethanol as extracting solvent, and directly diosgenin is extracted in dissolving.
The principle of extraction diosgenin proposed by the invention is: the 85%-95% ethanol of heat has bigger solubleness to diosgenin, is easy to diosgenin is extracted from yam water Jie thing.Contain a large amount of acidic resins and eggplant class pigment etc. in water Jie thing of diosgenin plant, this class impurity can form calcium salt with calcium hydroxide, and atomic to alcoholic acid solubleness, so can utilize calcium hydroxide to remove acidic resins.Wax in water Jie thing and chlorophyll etc. can be by being removed with activated carbon adsorption in acidic ethanol.Because of diosgenin to the dissolve with ethanol degree under the room temperature lower (diosgenin is about 5: 1 at the ratio of the solubleness in 95% ethanol under boiling point and the room temperature).Bigger than diosgenin to alcoholic acid solubleness, in spissated crystallisation process, △-Tigogenin etc. are stayed in the mother liquor morely and are not separated out, so can obtain the diosgenin of higher degree.
Because the present invention adopts ethanol to do to extract solvent, has overcome the defective of making to extract solvent with gasoline, has operational safety, technology is brief, the advantage that extraction yield is high.
Below in conjunction with embodiment the present invention is further described.
After conventional pressurized, heated hydrolysis in water Jie thing of the Chinese yam plant of gained (wherein diosgenin content is 4-8%), add calcium hydroxide, and it is even to add water concocting, three's amount ratio is 1: 0.1～0.2: 3～4(water Jie thing: calcium hydroxide: water), descended dry 4-8 hour at 95 ℃-105 ℃ then.Form dry.Dry is extracted twice with the heating of 85-95% alcohol reflux, and the total ethanol consumption is 15～30 times (volumes) of water Jie thing weight.Each all reflux 1 to 2 hour, filtered while hot is transferred pH value 1-6 with concentrated hydrochloric acid, adds activated carbon, and reheat refluxed 0.5 hour, and filtered while hot obtains the purified extracting solution.The purified extracting solution is concentrated under normal pressure or decompression, after being concentrated into 2～4 times of volumes of water Jie thing weight ratio, be statically placed in room temperature (10-30 ℃) 36-48 hour, leach the saponin crystallization, crystallize to neutrality with washing with alcohol, then, above-mentioned saponin product 95-105 ℃ of drying, can be got content and is the diosgenin more than 95%.
Another embodiment of the present invention is as follows: take by weighing yam water Jie thing 100 gram, add 20 gram calcium hydroxides and the blending of 400 ml waters evenly, 105 ℃ of dryings 4 hours.Dry extracts twice with the heating of 90% alcohol reflux, and consumption is 800,700 milliliters, all heats 1 hour, takes advantage of heat filtering.United extraction liquid transfers pH value to the acid 5 gram gacs that add with concentrated hydrochloric acid, refluxes the heat filter 0.5 hour.Be concentrated into 200 milliliters under the filtrate normal pressure, put in indoor (25 ℃) and leached the diosgenin crystallization in 36 hours, use washing with alcohol, crystallize to totally, 105 ℃ of dryings 2 hours are weighed, and survey fusing point and content (HPLE method mensuration).The result is as follows:
Claims (3)
1, a kind of method of extracting diosgenin from yam is characterized in that making to extract solvent with ethanol, and directly the diosgenin in the yam is extracted in dissolving.
2, the method for extraction diosgenin according to claim 1 is characterized in that the alcohol concn that extracts is 85-95%, and the temperature of crystallisation by cooling is 10 ℃ to 30 ℃.
3, the method for extraction diosgenin according to claim 1 is characterized in that extracting solution arrives pH value 1-6 with the hydrochloric acid acid adjustment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94104778A CN1061988C (en) | 1994-05-03 | 1994-05-03 | Method for extracting diosgenin from Dioscorea plant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94104778A CN1061988C (en) | 1994-05-03 | 1994-05-03 | Method for extracting diosgenin from Dioscorea plant |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1111250A true CN1111250A (en) | 1995-11-08 |
| CN1061988C CN1061988C (en) | 2001-02-14 |
Family
ID=5031747
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN94104778A Expired - Fee Related CN1061988C (en) | 1994-05-03 | 1994-05-03 | Method for extracting diosgenin from Dioscorea plant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1061988C (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1061985C (en) * | 1996-04-03 | 2001-02-14 | 中国科学院上海有机化学研究所 | Method for preparation of progestol by degradation of steroidal saponin |
| CN1091773C (en) * | 1999-06-27 | 2002-10-02 | 中国科学院昆明植物研究所 | Process for preparing yam saponin |
| CN100342858C (en) * | 2003-12-31 | 2007-10-17 | 天津市天士力制药股份有限公司 | Application of yam total saponin in the process for preparing anti-aspirin resisting medicine |
| CN100432095C (en) * | 2006-05-16 | 2008-11-12 | 郑州大学 | Waste-water-free production method for diosgenin |
| CN101402669B (en) * | 2008-11-19 | 2013-03-20 | 湖南科源生物制品有限公司 | Environment friendly method for producing diosgenin |
| CN103882086A (en) * | 2013-12-28 | 2014-06-25 | 赵长伟 | Extraction method of dioscorea composita saponin |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1033278A (en) * | 1987-11-24 | 1989-06-07 | 白求恩医科大学 | Technology for producing ginsenoside re monomer |
| CN1068657A (en) * | 1992-06-12 | 1993-02-03 | 湖南湘西制药厂 | Fast measuring method of dioscoreaceae saponin content |
-
1994
- 1994-05-03 CN CN94104778A patent/CN1061988C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1061985C (en) * | 1996-04-03 | 2001-02-14 | 中国科学院上海有机化学研究所 | Method for preparation of progestol by degradation of steroidal saponin |
| CN1091773C (en) * | 1999-06-27 | 2002-10-02 | 中国科学院昆明植物研究所 | Process for preparing yam saponin |
| CN100342858C (en) * | 2003-12-31 | 2007-10-17 | 天津市天士力制药股份有限公司 | Application of yam total saponin in the process for preparing anti-aspirin resisting medicine |
| CN100432095C (en) * | 2006-05-16 | 2008-11-12 | 郑州大学 | Waste-water-free production method for diosgenin |
| CN101402669B (en) * | 2008-11-19 | 2013-03-20 | 湖南科源生物制品有限公司 | Environment friendly method for producing diosgenin |
| CN103882086A (en) * | 2013-12-28 | 2014-06-25 | 赵长伟 | Extraction method of dioscorea composita saponin |
| CN103882086B (en) * | 2013-12-28 | 2016-06-29 | 赵长伟 | The extracting method of Dioscorea camposita Saponin |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1061988C (en) | 2001-02-14 |
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