CN103087143A - Method for extracting tigogenin from squeezed juice of sisal residue - Google Patents
Method for extracting tigogenin from squeezed juice of sisal residue Download PDFInfo
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- CN103087143A CN103087143A CN2013100067702A CN201310006770A CN103087143A CN 103087143 A CN103087143 A CN 103087143A CN 2013100067702 A CN2013100067702 A CN 2013100067702A CN 201310006770 A CN201310006770 A CN 201310006770A CN 103087143 A CN103087143 A CN 103087143A
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Abstract
The invention discloses a method for extracting tigogenin from squeezed juice of sisal residue. The method for extracting tigogenin from squeezed juice of sisal residue disclosed by the invention comprises the following steps: squeezing juice by squeezing fresh sisal residue to obtain squeezed juice of sisal; filtering by filtering the squeezed juice of sisal and removing coarse residue to obtain a coarse residue filter liquor; centrifuging by centrifuging the filter liquor to obtain a transparent liquor; fermenting by naturally fermenting the transparent liquor at normal temperatures to obtain a sisalagenin fermentation liquor; centrifuging by centrifuging the fermentation liquor to obtain a sisal paste; carrying out acidolysis by adding the sisal paste and concentrated sulfuric acid into a reaction kettle, heating and carrying out acidolysis on the sisalagenin; drying by neutralizing sulfuric acid in an acidolysis liquor by using calcium hydroxide, heating and drying in vacuum, and crushing to obtain powdery tigogenin crude product; and purifying by extracting the sisalagenin in crude saponin by using hot ethanol, filtering, concentrating and stewing in vacuum, centrifuging and collecting saponin crystals, heating and drying to obtain finished products of tigogenin. The tigogenin extracted by the method for extracting tigogenin from squeezed juice of sisal residue disclosed by the invention has the advantages of good quality, high purity, less energy consumption, simple process, high recovery rate, energy conservation, environmental friendliness and the like.
Description
Technical field
The present invention relates to a kind of extracting method, specifically a kind of squeezing the juice from sisal dregs extracted the method for tigogenin.
Background technology
Sisal hemp is called and is your fiber crops of western yarn, water silk fiber crops, sisal etc., the tongue the orchid family of being born in the year of dragon, and Agave contains the tigogenin (tigogenin) that the form with the steroid saponin aglucon exists, and its C3 position is connected with sugar chain by the saponin key with the C26 position.Prepare tigogenin, must the hydrolyzing saponin key.Contain multiple saponin(e in the sisal hemp juice of gained and sisal dregs when extracting fiber, main component is the steroidal saponin that can be hydrolyzed to tigogenin.Tigogenin has anti-inflammatory, analgesic, analgesia, strengthens immunity, reduces blood sugar, antitumor, anticancer, antibiotic, reducing blood-fat, the effect such as hypotensive, is widely used, and can be used as the precursor of synthesizing steroid medicine, synthetic more than 120 kind of hormone medicine; Also be widely used in the industries such as food, makeup and livestock industry.
At present, the production technique of domestic extraction tigogenin is all acid-hydrolysis method, and squeezing the juice of producing in the time of generally first will extracting fiber is stored in fermentation vat, spontaneous fermentation a couple of days to tens day, obtain numb cream after insoluble sisal hemp saponin(e natural subsidence, then dry, obtain impure a lot of dry numb cream.The at high temperature acidolysis of fiber crops cream obtains tigogenin.Because the impurity of numb cream is too many, cause the sulfuric acid that consumes also corresponding too many, the amount of the ethanol that follow-up purification procedures consumes is also very large, has significantly increased production cost.At first the present invention removes the impurity of sisal hemp juice with filtration, centrifugal method in the production technique of tigogenin, then process is less than the spontaneous fermentation of 24 hours, centrifugal collection because of its sugar chain Partial digestion after the sisal hemp saponin(e of water-soluble decline, shortened the production cycle of collecting the sisal hemp saponin(e, significantly reduced the content of impurity in the sisal hemp saponin(e, and then significantly reduce required sulfuric acid and the ethanol of operation such as follow-up acidolysis, purifying, reached the purpose that significantly reduces production costs.
China sisal hemp main producing region in Guangxi, the areas such as Guangdong and Hainan, the sisal hemp cultivated area in Guangxi is maximum at present.Sisal hemp has a large amount of sisal hemp juice after sisal fibers is extracted in processing, also be not developed at present.Abundant sisal hemp raw material resources are for industrialization of the present invention provides solid raw material guarantee.
Summary of the invention
Technical problem to be solved by this invention is to reduce the consumption of sulfuric acid and ethanol by the foreign matter content that reduces the sisal hemp saponin(e, and then reduces the production cost of tigogenin.
The present invention is achieved by the following technical programs:
A kind of squeezing the juice from sisal dregs extracted the method for tigogenin, and it comprises the steps:
(1) squeeze the juice, fresh sisal hemp meat slag is squeezed, obtain sisal hemp and squeeze the juice;
(2) filter, with the sisal hemp filtration of squeezing the juice, remove thick slag, obtain thick slag filtrate;
(3) centrifugal, filtrate is centrifugal, obtain containing the transparent liquid of sisal hemp saponin(e;
(4) fermentation, the spontaneous fermentation at normal temperatures of transparent liquid obtains containing the fermented liquid of the sisal hemp saponin(e of sugar chain Partial digestion;
(5) centrifugal, fermented liquid is carried out centrifugal collection sisal hemp saponin(e, obtain sisal hemp cream;
(6) acidolysis adds sisal hemp cream and the vitriol oil in reactor, heating acidolysis sisal hemp saponin(e;
(7) drying, with in calcium hydroxide and after the sulfuric acid of acid hydrolysis solution, vacuum and heating drying is pulverized, and obtains powdery tigogenin crude product;
(8) purifying, with the tigogenin in the thick saponin of hot ethanol extraction, filtered while hot, through vacuum concentration, standing, centrifugal collection saponin crystal obtains the tigogenin finished product after heat drying.
Preferably, described fresh sisal dregs is the sisal dregs after fiber.
Preferably, the filtration that is filtered into employing 200 order filter clothes of described step (2).
Preferably, the centrifugal of described step (3) and (5) is centrifugal with disk plate centrifuge, and rotating speed is 5000～8000 rev/mins.
Preferably, the fermentation of described step (4) is in temperature being spontaneous fermentation 12～24 hours under the condition of 15 ℃～25 ℃.
Preferably, the acidity of the acidolysis of described step (6) is that final concentration is the sulfuric acid of 2～3mol/L, and Heating temperature is 120～130 ℃.
Preferably, the purifying of described step (8), the ratio of thick saponin and ethanol is 1: 10～1: 30, alcohol concn is 95%.
At first remove the impurity of sisal hemp juice with filtration, centrifugal method in the production technique of tigogenin, then process is less than the spontaneous fermentation of 24 hours, centrifugal collection because of its sugar chain Partial digestion after the sisal hemp saponin(e of water-soluble decline, shortened the production cycle of collecting the sisal hemp saponin(e, significantly reduced the content of impurity in the sisal hemp saponin(e, and then significantly reduce required sulfuric acid and the ethanol of operation such as follow-up acidolysis, purifying, reached the purpose that significantly reduces production costs.
Beneficial effect of the present invention is: tigogenin quality better, the purity extracted by tigogenin production technique of the present invention are high, produce less energy intensive, have significantly reduced the consumption of sulfuric acid, ethanol.Compare with traditional production technique, at the bottom of having production cost, the rate of recovery is high, the advantages such as energy-conserving and environment-protective.
Embodiment
The present invention is described in further detail below in conjunction with embodiment, but embodiments of the present invention are not limited to the scope that embodiment represents.
Embodiment 1
To extract the remaining fresh sisal dregs squeezing of sisal fibers through processing, and obtain sisal hemp and squeeze the juice.Squeeze the juice with 200 order filter-cloth filtering sisal hemps, remove thick slag, obtain thick slag filtrate.With disk plate centrifuge centrifugal (5000 rev/mins) filtrate, obtain containing the clear solution of sisal hemp saponin(e.Allow transparent liquid normal temperature (25 ℃) in fermentation vat descend spontaneous fermentation 12 hours, obtain the fermented liquid of the sisal hemp saponin(e of sugary chain portion enzymolysis.With the centrifugal collection sisal hemp of disk plate centrifuge centrifugal (7000 rev/mins) saponin(e, obtain sisal hemp cream.Add sisal hemp cream and the vitriol oil (final concentration of sulfuric acid is 2mol/L) in reactor, heat to 121 ℃, 121 ℃ of constant temperature 2 hours, acidolysis sisal hemp saponin(e obtains containing the acid hydrolysis solution of tigogenin.With in calcium hydroxide and the sulfuric acid of acid hydrolysis solution to pH6.0, through vacuum and heating drying, pulverize, obtain powdery tigogenin crude product.Be the ratio of 1: 20 in the ratio of thick saponin and ethanol, extract tigogenin in thick saponin with 95 ℃ of hot ethanols (concentration is 95% industrial alcohol), filtered while hot, to 8% of original volume, standing through vacuum concentration, oversaturated tigogenin is separated out.With the centrifugal collection of atresia tripod pendulum type batch centrifugal saponin crystal, obtain the tigogenin finished product after heat drying (105 ℃).
Embodiment 2
To extract the remaining fresh sisal dregs squeezing of sisal fibers through processing, and obtain sisal hemp and squeeze the juice.Squeeze the juice with 200 order filter-cloth filtering sisal hemps, remove thick slag, obtain thick slag filtrate.With disk plate centrifuge centrifugal (6000 rev/mins) filtrate, obtain containing the clear solution of sisal hemp saponin(e.Allow transparent liquid normal temperature (32 ℃) in fermentation vat descend spontaneous fermentation 8 hours, obtain the fermented liquid of the sisal hemp saponin(e of sugary chain portion enzymolysis.With the centrifugal collection sisal hemp of disk plate centrifuge centrifugal (7000 rev/mins) saponin(e, obtain sisal hemp cream.Add sisal hemp cream and the vitriol oil (final concentration of sulfuric acid is 2.5mol/L) in reactor, heat to 125 ℃, 125 ℃ of constant temperature 2.5 hours, acidolysis sisal hemp saponin(e obtains containing the acid hydrolysis solution of tigogenin.With in calcium hydroxide and the sulfuric acid of acid hydrolysis solution to pH5.0, through vacuum and heating drying, pulverize, obtain powdery tigogenin crude product.It is the ratio of 1: 25 in the ratio of thick saponin and ethanol, extract tigogenin in thick saponin with 95 ℃ of hot ethanols (concentration is 95% food grade ethanol), filtered while hot, through vacuum concentration to 9% of original volume, standing, oversaturated tigogenin is separated out.With the centrifugal collection of atresia tripod pendulum type batch centrifugal saponin crystal, obtain the tigogenin finished product after heat drying (110 ℃).
Embodiment 3
To extract the remaining fresh sisal dregs squeezing of sisal fibers through processing, and obtain sisal hemp and squeeze the juice.Squeeze the juice with 200 order filter-cloth filtering sisal hemps, remove thick slag, obtain thick slag filtrate.With disk plate centrifuge centrifugal (7000 rev/mins) filtrate, obtain containing the clear solution of sisal hemp saponin(e.Allow transparent liquid normal temperature (18 ℃) in fermentation vat descend spontaneous fermentation 24 hours, obtain the fermented liquid of the sisal hemp saponin(e of sugary chain portion enzymolysis.With the centrifugal collection sisal hemp of disk plate centrifuge centrifugal (7000 rev/mins) saponin(e, obtain sisal hemp cream.Add sisal hemp cream and the vitriol oil (final concentration of sulfuric acid is 3mol/L) in reactor, heat to 130 ℃, 130 ℃ of constant temperature 3 hours, acidolysis sisal hemp saponin(e obtains containing the acid hydrolysis solution of tigogenin.With in calcium hydroxide and the sulfuric acid of acid hydrolysis solution to pH7, through vacuum and heating drying, pulverize, obtain powdery tigogenin crude product.It is the ratio of 1: 18 in the ratio of thick saponin and ethanol, extract tigogenin in thick saponin with 95 ℃ of hot ethanols (concentration is 95% food grade ethanol), filtered while hot, through vacuum concentration to 8.5% of original volume, standing, oversaturated tigogenin is separated out.With the centrifugal collection of atresia tripod pendulum type batch centrifugal saponin crystal, obtain the tigogenin finished product after vacuum and heating drying (105 ℃).
Although embodiment of the present invention are open as above, but it is not restricted to listed utilization in specification sheets and embodiment, it goes for various suitable the field of the invention fully, for those skilled in the art, can easily realize other modification, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the example of describing.
Claims (7)
1. squeeze the juice from sisal dregs and extract the method for tigogenin for one kind, it is characterized in that, it comprises the steps:
(1) squeeze the juice, fresh sisal hemp meat slag is squeezed, obtain sisal hemp and squeeze the juice;
(2) filter, with the sisal hemp filtration of squeezing the juice, remove thick slag, obtain thick slag filtrate;
(3) centrifugal, filtrate is centrifugal, obtain containing the transparent liquid of sisal hemp saponin(e;
(4) fermentation, the spontaneous fermentation at normal temperatures of transparent liquid obtains containing the fermented liquid of the sisal hemp saponin(e of sugar chain Partial digestion;
(5) centrifugal, fermented liquid is carried out centrifugal collection sisal hemp saponin(e, obtain sisal hemp cream;
(6) acidolysis adds sisal hemp cream and the vitriol oil in reactor, heating acidolysis sisal hemp saponin(e;
(7) drying, with in calcium hydroxide and after the sulfuric acid of acid hydrolysis solution, vacuum and heating drying is pulverized, and obtains powdery tigogenin crude product;
(8) purifying, with the tigogenin in the thick saponin of hot ethanol extraction, filtered while hot, through vacuum concentration, standing, centrifugal collection saponin crystal obtains the tigogenin finished product after heat drying.
According to claim 1 from sisal hemp is squeezed the juice the method for extraction tigogenin, it is characterized in that, described fresh sisal dregs is the sisal dregs after fiber.
3. according to claim 1 squeezing the juice from sisal hemp extracted the method for tigogenin, it is characterized in that the filtration that is filtered into employing 200 order filter clothes of described step (2).
4. according to claim 1 squeezing the juice from sisal hemp extracted the method for tigogenin, it is characterized in that, the centrifugal of described step (3) and (5) is centrifugal with disk plate centrifuge, and rotating speed is 5000～8000 rev/mins.
5. according to claim 1 squeezing the juice from sisal hemp extracted the method for tigogenin, it is characterized in that, the fermentation of described step (4) is in temperature being spontaneous fermentation 12～24 hours under the condition of 15 ℃～25 ℃.
6. according to claim 1 squeezing the juice from sisal hemp extracted the method for tigogenin, it is characterized in that, the acidity of the acidolysis of described step (6) is that final concentration is the sulfuric acid of 2～3mol/L, and Heating temperature is 120～130 ℃.
7. according to claim 1 squeezing the juice from sisal hemp extracted the method for tigogenin, it is characterized in that, and the purifying of described step (8), the ratio of thick saponin and ethanol is 1: 10～1: 30, alcohol concn is 95%.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103834713A (en) * | 2013-12-19 | 2014-06-04 | 广西大学 | Extraction method for 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 |
| CN104211481A (en) * | 2014-09-24 | 2014-12-17 | 广西众益生物科技有限公司 | Compound fertilizer containing tigogenin extracted residue |
| CN105506051A (en) * | 2015-12-23 | 2016-04-20 | 北京颐方生物科技有限公司 | Method for extracting tigogenin and/or hecogenin with composite bacteria method |
| CN105796775A (en) * | 2016-03-31 | 2016-07-27 | 天峨县平昌生态农业有限公司 | Production method for sisal hemp paste |
| CN109232709A (en) * | 2018-10-31 | 2019-01-18 | 石门红太阳生物科技有限公司 | A method of extracting high-purity tigogenin from sisal dregs |
| CN109295151A (en) * | 2018-10-31 | 2019-02-01 | 石门红太阳生物科技有限公司 | A kind of tigogenin extract in sisal hemp cream produce fermentation process |
| CN110642917A (en) * | 2019-10-01 | 2020-01-03 | 石门红太阳生物科技有限公司 | Novel extraction equipment and extraction method for tigogenin |
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| CN1068121A (en) * | 1992-01-20 | 1993-01-20 | 广西南宁制药企业集团公司 | The process for extracting of Tigogenin |
| CN1528782A (en) * | 2003-10-09 | 2004-09-15 | 滕明星 | Sisal hemp steroid hormone production method |
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2013
- 2013-01-09 CN CN2013100067702A patent/CN103087143A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1068121A (en) * | 1992-01-20 | 1993-01-20 | 广西南宁制药企业集团公司 | The process for extracting of Tigogenin |
| CN1528782A (en) * | 2003-10-09 | 2004-09-15 | 滕明星 | Sisal hemp steroid hormone production method |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103834713B (en) * | 2013-12-19 | 2016-03-16 | 广西大学 | A kind of extracting method of tigogenin |
| CN103834713A (en) * | 2013-12-19 | 2014-06-04 | 广西大学 | Extraction method for 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 |
| CN104211481B (en) * | 2014-09-24 | 2017-04-19 | 广西众益生物科技有限公司 | Compound fertilizer containing tigogenin extracted residue |
| CN104211481A (en) * | 2014-09-24 | 2014-12-17 | 广西众益生物科技有限公司 | Compound fertilizer containing tigogenin extracted residue |
| CN105506051A (en) * | 2015-12-23 | 2016-04-20 | 北京颐方生物科技有限公司 | Method for extracting tigogenin and/or hecogenin with composite bacteria method |
| CN105506051B (en) * | 2015-12-23 | 2018-08-10 | 北京颐方生物科技有限公司 | Compound bacteria method extracts tigogenin and/or the method for Hai Kejining |
| CN105796775A (en) * | 2016-03-31 | 2016-07-27 | 天峨县平昌生态农业有限公司 | Production method for sisal hemp paste |
| CN105796775B (en) * | 2016-03-31 | 2019-10-15 | 天峨县平昌生态农业有限公司 | A kind of production method of sisal hemp fiber crops cream |
| CN109232709A (en) * | 2018-10-31 | 2019-01-18 | 石门红太阳生物科技有限公司 | A method of extracting high-purity tigogenin from sisal dregs |
| CN109295151A (en) * | 2018-10-31 | 2019-02-01 | 石门红太阳生物科技有限公司 | A kind of tigogenin extract in sisal hemp cream produce fermentation process |
| CN110642917A (en) * | 2019-10-01 | 2020-01-03 | 石门红太阳生物科技有限公司 | Novel extraction equipment and extraction method for tigogenin |
| CN110642917B (en) * | 2019-10-01 | 2023-07-28 | 石门红太阳生物科技有限公司 | Novel extraction equipment and extraction method of tigogenin |
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Application publication date: 20130508 |