CN103087143A - Method for extracting tigogenin from squeezed juice of sisal residue - Google Patents

Method for extracting tigogenin from squeezed juice of sisal residue Download PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
tigogenin
sisal
sisal hemp
juice
saponin
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.)
Pending
Application number
CN2013100067702A
Other languages
Chinese (zh)
Inventor
彭胜良
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
GUANGXI NANJIAN BIOTECHNOLOGY CO Ltd
Original Assignee
GUANGXI NANJIAN BIOTECHNOLOGY CO Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by GUANGXI NANJIAN BIOTECHNOLOGY CO Ltd filed Critical GUANGXI NANJIAN BIOTECHNOLOGY CO Ltd
Priority to CN2013100067702A priority Critical patent/CN103087143A/en
Publication of CN103087143A publication Critical patent/CN103087143A/en
Pending legal-status Critical Current

Links

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

A kind of squeezing the juice from sisal dregs extracted the method for tigogenin
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%.
CN2013100067702A 2013-01-09 2013-01-09 Method for extracting tigogenin from squeezed juice of sisal residue Pending CN103087143A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2013100067702A CN103087143A (en) 2013-01-09 2013-01-09 Method for extracting tigogenin from squeezed juice of sisal residue

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2013100067702A CN103087143A (en) 2013-01-09 2013-01-09 Method for extracting tigogenin from squeezed juice of sisal residue

Publications (1)

Publication Number Publication Date
CN103087143A true CN103087143A (en) 2013-05-08

Family

ID=48200314

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2013100067702A Pending CN103087143A (en) 2013-01-09 2013-01-09 Method for extracting tigogenin from squeezed juice of sisal residue

Country Status (1)

Country Link
CN (1) CN103087143A (en)

Cited By (7)

* Cited by examiner, † Cited by third party
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

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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 (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103834713A (en) * 2013-12-19 2014-06-04 广西大学 Extraction method for tigogenin
CN103834713B (en) * 2013-12-19 2016-03-16 广西大学 A kind of extracting 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
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
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
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

Similar Documents

Publication Publication Date Title
CN103087143A (en) Method for extracting tigogenin from squeezed juice of sisal residue
CN103834713B (en) A kind of extracting method of tigogenin
CN101503433B (en) Preparation of plant source glucosamine hydrochloride
CN104774887A (en) Preparation method of corncob xylooligosaccharide
CN101191136A (en) Clean producing technique for extracting saponin from turmeric and coproducing fuel ethanol
CN102634612B (en) Method for producing high-purity L-arabinose by using bagasse pith as raw materials
CN103641930B (en) A kind of method utilizing enzyme process to extract pectin from pineapple peel, slag
CN102030630A (en) Method for producing industrial grade sodium gluconate or calcium gluconate from yellow ginger starch
CN101864000A (en) Pectin extraction method from waste sisal dregs
CN106146686A (en) A kind of technique utilizing Receptaculum Helianthi industrialized production pectin
CN102584571A (en) Extraction process for shikimic acid in fermentation liquor
CN102618609A (en) Method for comprehensively utilizing degreased rice bran
CN104341538B (en) A kind of method for separating and preparing of high HG content Helianthi pectin
CN102382911A (en) Method for preparing crystalline xylose by using bagasse pith as raw material
CN102399303A (en) Extraction method of pectin
CN101891774B (en) Production process of rhamnose
CN102180921A (en) Method for extracting high-purity rutin from boxthorn leaves
CN102464700B (en) Hydrolysis extraction process for yam diosgenin
CN100532396C (en) Process for preparing high purity pectin by using apple pomace
CN103059158A (en) Method for inhibiting foam generation in tea flower polysaccharide extraction
CN101816372A (en) Clean production method of coproduced biologic protein feed of diosgenin
CN105237339A (en) Method for extracting octacosanol by using sugar refinery mixing juice floating residue as raw material
CN102660619A (en) Method for clean production of saponin from Dioscorea zingiberensis C. H. Wright
CN109160935B (en) Method for extracting tigogenin and cellulose
CN105907801A (en) Method of continuously producing dietary fibers, alcohol and single-cell protein with potato residue

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C12 Rejection of a patent application after its publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20130508