CN1068121A - The process for extracting of Tigogenin - Google Patents
The process for extracting of Tigogenin Download PDFInfo
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- CN1068121A CN1068121A CN 92100484 CN92100484A CN1068121A CN 1068121 A CN1068121 A CN 1068121A CN 92100484 CN92100484 CN 92100484 CN 92100484 A CN92100484 A CN 92100484A CN 1068121 A CN1068121 A CN 1068121A
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- tigogenin
- raw material
- saponification
- hydrolysis
- sisal hemp
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Abstract
The present invention proposes the process for extracting that a kind of Tigogenin is a tigogenin.The characteristics of this technology are to get juice from the sisal hemp waste residue in east that removes fiber, through fermentation, hydrolysis, saponification, extraction, dewaxing and decolorization, concentrate, crystallization, oven dry and get.This processing method cost is low, the yield height, and quality is good, and raw material sources are wide, turn waste into wealth, and comprehensive utilization is for development and use steroid hormone medicine provides a kind of new raw material resources.
Description
The present invention relates to a kind of process for extracting of process for extracting, especially Tigogenin of natural resource of steroid hormone class medicine.
Tigogenin (Tigogenin, trade(brand)name tigogenin) formal name used at school: 5a, 25D-spirostane-3 β hydroxyl, it and diosgenin (Diosgenin), hecogenin (Hecogenin) are all important steroid hormone raw material.The raw material potato of diosgenin is a wild plant, resource-constrained; The american aloe of hecogenin is the kind that eliminate gradually on the farm because of producing the fiber rate low also; And the sisal hemp in east produces fiber rate height, and fiber is long, is the cash crop of a large amount of plantations of China's southern farm, the resource abundance.Tigogenin extracts from the dried slag of sisal hemp in east that removes fiber, replace other saponin that resource peters out and become trend, and higher with tigogenin synthesizing efficient cortin yield, cost is lower, demonstrates bigger superiority.
The objective of the invention is for development and use steroid hormone medicine provides a kind of new raw material resources, and be that a kind of cost is low, yield is high, the measured process for extracting that is suitable for the Tigogenin of industrialness production of matter.
Operational path of the present invention is seen accompanying drawing.
Production process of the present invention is:
1, the preparation of the dried slag of sisal hemp in east:
The dried slag of sisal hemp is the starting raw material that enters the factory-prepared tigogenin, and the preparation of the dried slag of sisal hemp is to finish in the raw material site on farm.Get the bright numb meat waste residue that the raw material site has been removed fiber, get numb juice through squeezing, put in the pond open-air spontaneous fermentation sedimentation after 10～15 days, supernatant liquid bleeds off, sediment put the sunning ground after drying the dried slag of sisal hemp.
4 tons of the sisal hemp leaf average yield per mus in east of the annual harvesting in farm, sisal hemp leaf per ton goes the bright numb meat waste residue compressible behind the fiber to get numb water 0.5M
3, every 1M
3Fiber crops water sediment after fermenting dries and can get 10～15 kilograms of the dried slags of sisal hemp.
2, the preparation of tigogenin:
A, hydrolysis
Material ratio: the dried slag of sisal hemp: water: the vitriol oil: lime=1: 45: 0.5: 0.1
Water is dropped into hydrolytic decomposition pot according to quantity, add sulfuric acid then lentamente and make and become 2 equivalents, drop into sealed cans mouth behind the dried slag of sisal hemp again.Stir and steam heating, temperature is 130 ℃～142 ℃ in the control, interior pressure 2.5～3kg/cm
2Discharging is finished in reaction, puts whizzer and gets rid of and wash hydrolyzate to neutral.Add lime mixing furnishing pasty state in the hydrolyzate, tray send dry back to be the saponification hydrolyzate.The hydrolyzate yield is that 60～70%(connects lime heavily).
B, extraction
Material ratio: hydrolyzate: alcohol: concentrated hydrochloric acid: gac=1: 15: an amount of: 0.2
Saponification posthydrolysis thing alcoholic extraction secondary.Make with the heating of 10 times of amount 95% alcohol for the first time and refluxed 1 hour; Reflux filtered while hot half an hour with 5 times of amounts for the second time.Twice extract merges, and transferring PH with concentrated hydrochloric acid is 5, adds gac, reflux 1 hour, heat filter.Filtrate send concentration tank dense surplus 1: 4 volume.Concentrated solution is cooled to about 25 ℃ to be placed crystallization and spends the night.Leach crystal, it is neutral colourless only to be washed till washing lotion with alcohol.Promptly get tigogenin after the crystal drying, be Tigogenin.Yield is that 3～6.6%(is to the dried slag meter of sisal hemp), content is more than 85%, fusing point: 196～206 ℃.
Extraction process cost of the present invention is low, yield is high, and quality is good, and raw material sources are wide, turn waste into wealth, and comprehensive utilization is for development and use steroid hormone medicine provides a kind of new raw material resources.
Embodiment:
Get the bright dregs of linseeds or sesame seeds that the raw material site has been removed fiber, get its juice through squeezing machine squeezing, it is surplus to put in the pond open-air spontaneous fermentation sedimentation first quarter moon, and supernatant liquid discards, and sediment is put the sunning ground and dried and get final product.
In hydrolytic decomposition pot, add 900L water and 200 kilograms of sulfuric acid.Stir evenly (measure the sulfuric acid equivalent and should be 2N, should drink when not enough add to foot) slightly, seal after dropping into 200 kilograms of dried slags of sisal hemp, start and stir and jacket steam, heating makes 135 ℃, interior pressure 2.5kg/cm
2The time hydrolysis 2 hours, hydrolyzate is pressed in the container for storing liquid, change the whizzer inner filtration in batches, be washed to neutrality, take out hydrolyzate, in mixing machine, add calcium hydroxide and be mixed into pasty state for 20 kilograms, go into the drying room drying and dehydrating in the immigration dish.Weigh after doing 120～140 kilograms of hydrolyzates (comprising calcium hydroxide).
Hydrolyzate is dropped into extractor add alcohol 1000L, being heated to and boiling backflow after 1 hour, blowing makes extracting solution change in the bleacher by the insulation pressure-filtering tank.Add for the second time 500L alcohol reflux equally the back by pressure-filtering tank make filtered till.Twice extract adds 25 kilograms of hydrochloric acid 4L and gacs in bleacher, reflux 1 hour takes advantage of hot discharging to enter concentration tank by the insulation pressure-filtering tank, steams alcohol 600L, makes and extracts till the dense extremely about 800L of destainer.Take advantage of heat that concentrated solution is sent into crystallizer.
Concentrated solution is put into behind the crystallizer interlayer feed the cold water cooling and be cooled to room temperature, leave standstill and move into whizzer after 24 hours and filter, it is colourless only to be washed till washing lotion with an amount of alcohol.Send the drying room drying in the finished product immigration dish.Get tigogenin more than 9 kilograms, content 85%, fusing point: 196～206 ℃.
Claims (5)
1, a kind of process for extracting of Tigogenin is characterized in that: to the east of the waste residue of a sisal hemp be raw material, through press extracting juice, fermentation sedimentation, dry, acid hydrolysis, saponification, extract, go cured decolouring, concentrate, technologies such as crystallization, drying make.
2, the method for claim 1 is characterized in that raw material is removing the numb meat slag behind the fiber, to press extracting juice to produce throw out after spontaneous fermentation, its precipitation drying and getting.
3, the method for claim 1, the hydrolysis that it is characterized in that the dried slag of sisal hemp is with 5 times of volumes, 2 normal sulfuric acid, 130～142 ℃ of interior temperature, interior pressure 2.5～3kg/cm
2Hydrolysis is 2 hours under the condition.
4, the method for claim 1 is characterized in that the lime saponification of 20% amount that adds in the hydrolyzate, dries behind the furnishing pasty state.
5, the method for claim 1 is characterized in that hydrolyzate after the saponification with alcohol heating and refluxing extraction secondary, filters, and merges extract, and transferring PH with hydrochloric acid is 5, adds gac and refluxes 1 hour, the heat filter.Filtrate concentrates, cooling crystallization.To neutral, get product with the alcohol washing after the drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92100484 CN1068121A (en) | 1992-01-20 | 1992-01-20 | The process for extracting of Tigogenin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92100484 CN1068121A (en) | 1992-01-20 | 1992-01-20 | The process for extracting of Tigogenin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1068121A true CN1068121A (en) | 1993-01-20 |
Family
ID=4938610
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92100484 Pending CN1068121A (en) | 1992-01-20 | 1992-01-20 | The process for extracting of Tigogenin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1068121A (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1036997C (en) * | 1993-07-01 | 1998-01-14 | 广西壮族自治区南宁制药企业集团公司 | Process for extracting and separating high content "tikejining" |
| CN1049662C (en) * | 1997-06-28 | 2000-02-23 | 陕西省中国科学院植物化学工程中心 | Method for extracting steroid saponin from trigonella foenum graecum seed |
| 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 |
| CN100363379C (en) * | 2005-09-22 | 2008-01-23 | 王锦军 | Process for producing high purity hecogenin and tigogenin |
| CN100370991C (en) * | 2006-04-06 | 2008-02-27 | 成都厚发科技开发有限公司 | Pharmaceutical composition with anti-inflammation action |
| CN101838343A (en) * | 2010-04-29 | 2010-09-22 | 广西大学 | Method for preparing pectin by using waste sisal dregs |
| CN101560240B (en) * | 2009-05-18 | 2011-12-14 | 广西福园剑麻股份有限公司 | Extracting method of ticogenin with high yield |
| CN103087143A (en) * | 2013-01-09 | 2013-05-08 | 广西南剑生物科技有限公司 | Method for extracting tigogenin from squeezed juice of sisal residue |
| CN103102386A (en) * | 2013-02-20 | 2013-05-15 | 广西万德药业股份有限公司 | Preparation method of Tigogenin |
| CN104109186A (en) * | 2014-06-12 | 2014-10-22 | 广西众益生物科技有限公司 | Purifying method of ticogenin crude product |
| CN110590900A (en) * | 2019-09-29 | 2019-12-20 | 石门红太阳生物科技有限公司 | Dewaxing method in sisal hemp saponin production |
-
1992
- 1992-01-20 CN CN 92100484 patent/CN1068121A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1036997C (en) * | 1993-07-01 | 1998-01-14 | 广西壮族自治区南宁制药企业集团公司 | Process for extracting and separating high content "tikejining" |
| 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 |
| CN1049662C (en) * | 1997-06-28 | 2000-02-23 | 陕西省中国科学院植物化学工程中心 | Method for extracting steroid saponin from trigonella foenum graecum seed |
| CN100363379C (en) * | 2005-09-22 | 2008-01-23 | 王锦军 | Process for producing high purity hecogenin and tigogenin |
| CN100370991C (en) * | 2006-04-06 | 2008-02-27 | 成都厚发科技开发有限公司 | Pharmaceutical composition with anti-inflammation action |
| CN101560240B (en) * | 2009-05-18 | 2011-12-14 | 广西福园剑麻股份有限公司 | Extracting method of ticogenin with high yield |
| CN101838343A (en) * | 2010-04-29 | 2010-09-22 | 广西大学 | Method for preparing pectin by using waste sisal dregs |
| CN103087143A (en) * | 2013-01-09 | 2013-05-08 | 广西南剑生物科技有限公司 | Method for extracting tigogenin from squeezed juice of sisal residue |
| CN103102386A (en) * | 2013-02-20 | 2013-05-15 | 广西万德药业股份有限公司 | Preparation method of Tigogenin |
| CN103102386B (en) * | 2013-02-20 | 2015-10-28 | 广西万德药业股份有限公司 | The preparation method of tigogenin |
| CN104109186A (en) * | 2014-06-12 | 2014-10-22 | 广西众益生物科技有限公司 | Purifying method of ticogenin crude product |
| CN110590900A (en) * | 2019-09-29 | 2019-12-20 | 石门红太阳生物科技有限公司 | Dewaxing method in sisal hemp saponin production |
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