CN102351936A - Method for extracting ecdysterone from plant - Google Patents
Method for extracting ecdysterone from plant Download PDFInfo
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- CN102351936A CN102351936A CN201110264182XA CN201110264182A CN102351936A CN 102351936 A CN102351936 A CN 102351936A CN 201110264182X A CN201110264182X A CN 201110264182XA CN 201110264182 A CN201110264182 A CN 201110264182A CN 102351936 A CN102351936 A CN 102351936A
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Abstract
The invention discloses a method for extracting ecdysterone from a plant, which is characterized by comprising the following steps of: a, grinding a raw material, adding biological enzyme, performing enzymolysis at the temperature of between 40 and 50 DEG C for 2 to 3 hours, adding water, raising the temperature to be between 70 and 80 DEG C, preserving heat, soaking for 1 to 2 hours, extracting for two to three times, and filtering to obtain extract; and b, adding an ultrafiltration membrane into the extract for ultrafiltration, adding a nanofiltration membrane into permeate for concentrating, adding ethanol solution with the same volume as concentrated solution into the concentrated solution for filtering, adding ethyl acetate for extracting, adding activated carbon into raffinate for reflux decolorization, filtering and concentrating decolorized solution until ethanol is not crystallized, and drying crystals to obtain the ecdysterone. The method is easy to operate, high in extraction efficiency, low in energy consumption and suitable for industrial production.
Description
Technical field
The present invention relates to a kind of method of from plant, extracting ecdysterone, particularly relate to a kind of method that adopts enzymolysis and membrane filtration technique from plant, to extract ecdysterone.
Background technology
Ecdysterone is moulting hormone again.The fifties scientist from silkworm pupa purifying and two kinds of active substances, can induce insect molting, thereby be called as α-moulting hormone and β-moulting hormone.Now from 1000 various plants, isolated the analogue of many moulting hormones, Chinese yunnan is economized and from plants such as one hundred days green grass or young crops, is obtained a large amount of plant ecdysterones from Root of Willowleaf Achyranthes, Zhejiang Province from Radix Cyanotis vagae, Jiangsu Province.What effect the plant ecdysterone plays in plant not clear.If from plant and insect relation, the plant ecdysterone belongs to a kind of protective substance, can promote that larva casts off a skin early, turns to adult, avoid the larva of insect too much to invade the food plant.In Chinese Jiangsu, Zhejiang one band area of breeding silkworms, get the mulberry leaf of food when not enough when silkworm, from plant, extract ecdysterone and can be sprayed onto on the five age silkworm healths, promote silkworm suffixation of a nonsyllabic "r" pupa.
Discover that ecdysterone not only triggers insect, the beginning of the process of casting off a skin of Crustacean, and can guarantee the whole process of casting off a skin continue carry out, and promote new steps such as tanning of epidermis.Impel the new exterior skin of insect secretion; The formation of new entocuticle; The generation of moulting fluid; The digestion of old exterior skin; The dissolving of the old and new's cortex, separation, old epidermis is sloughed off, the expansion of new epidermis; The steps such as thickening of tanning and entocuticle, and the secretory activity of moulting hormone just in time reached the climax in the process of casting off a skin in the past.Ecdysterone not only is used in aquaculture widely, also can be used as sterilant and makeup and medicines and health protection aspect.
Plant ecdysterone process for extracting adopts water extraction or ethanol-extracted more, and concentrated solution adopts extraction or resin isolation, adopts aluminum oxide or silica gel to separate again.Traditional technology is: Radix Cyanotis vagae pulverizing → ethanol or water refluxing extraction → spissated medicinal extract is gone up alumina column separation → condensing crystal after adopting ethanol or ethanol, ethyl acetate mixture dissolving → concentrated once more upward alumina column or n-butanol extraction again.Document " extracts purifying β-moulting hormone technical study " from Radix Cyanotis vagae disclosed method is that Radix Cyanotis vagae is a raw material, use water extraction, adds Amberlyst process separation behind the finings, through recrystallization, isolates β-moulting hormone.Like patent (application number: 201010039119.1) " a kind of method and moulting hormone thereof that from blackspiked lovegrass herb with root, extracts moulting hormone "; This patent disclosed method be blackspiked lovegrass herb with root water carry or alcohol extracting after; Be evaporated to the liquid of relative density 1.05～1.20; With adjusting PH with base to 6～10; Use n-butanol again: ethyl acetate is 4: 6～0.5: 9.5 mixed extractant solvent; Through washing; And to be evaporated to relative density be 1.2～1.3 liquid extract; Cross strong basic type anion-exchange resin after adding 50～95% methyl alcohol or ethanol dissolved dilution, concentrating also through wash-out, decompression, drying under reduced pressure promptly gets described moulting hormone.As stated, existing technology exists the energy consumption height, extraction yield is low, technological operation is loaded down with trivial details and many technological deficiencies such as production cost height.
Summary of the invention
The objective of the invention is to overcome the deficiency and the technological deficiency of existing method, a kind of method of from plant, extracting ecdysterone is provided.
The objective of the invention is to realize through following technical scheme: a kind of method of from plant, extracting ecdysterone is characterized in that following steps:
A. raw material pulverizing adds biological enzyme after under the 40-50 ℃ of condition enzymolysis 2-3 hour, adds water and is warming up to 70-80 ℃, and insulation was soaked 1-2 hour, extracted 2-3 time, crosses and filters extracting solution;
B. said extracted liquid adds the ultra-filtration membrane ultrafiltration, adds nanofiltration membrane again through liquid and concentrates, and concentrated solution adds the equal-volume ethanolic soln and filters; Add ethyl acetate extraction again; Raffinate adds the gac reflux decolour, and destainer filters and is concentrated into no pure crystallization, the dry ecdysterone that gets of crystallisate.
The optional Commelianaceae tabasheer of raw material among described step a Radix Cyanotis vagae, labiate japanese bugle herb and amaranthaceous plant Root of Willowleaf Achyranthes.
Biological enzyme among the described step a is a kind of or arbitrary combination in cellulase, amylase and the polygalacturonase, and consumption is the 1-3 ‰ of material quantity.
Ultra-filtration membrane among the described step b is the hollow cellulose ultra-filtration membrane of molecular weight cut-off 2000-5000, and nanofiltration membrane is the hollow cellulose nanofiltration membrane of molecular weight cut-off 100-300.
Positively effect of the present invention is:
(1) method has been destroyed organization structure of the plant through adding the biological enzyme enzymolysis, and the easy stripping of effective constituent reduces and extracts temperature, has reduced the destruction of high temperature to effective constituent, has also reduced energy consumption;
(2) method adopts membrane filtration technique to carry out molecular retention, belongs to physical method, carries out under the normal temperature, has promptly realized removal of impurities, has concentrated material again, does not cause composition to decompose in the process, and simple to operate, power consumption is few.
Embodiment
To combine embodiment to further specify the present invention below.
Embodiment 1:
Commelianaceae tabasheer Radix Cyanotis vagae is pulverized; Get 10kg and add extractor; Taking by weighing the 30g cellulase is dissolved in the aqueous solution of 10kgph5 and adds extractor; Enzymolysis is after 2 hours under 50 ℃ of conditions; Be warming up to 80 ℃; Adding the 60kg insulation again soaked 2 hours; Filter liquide adds 50kg water insulation 1 hour again; Filter the hollow cellulose ultra-filtration membrane ultrafiltration of extracting solution adding molecular weight cut-off 2000; The hollow cellulose nanofiltration membrane that adds molecular weight cut-off 300 through liquid again concentrates; Get concentrated solution, add equal-volume 95% ethanolic soln and filter, add the equal-volume ethyl acetate extraction again 1 time; Raffinate adds 50g gac reflux decolour; Destainer filters and is concentrated into no pure crystallization, and crystallisate leaches the dry ecdysterone 126g of getting, content 87%.
Embodiment 2:
The labiate japanese bugle herb is pulverized; Get 10kg and add extractor; Taking by weighing 20g amylase is dissolved in the aqueous solution of 10kgph4 and adds extractor; Enzymolysis is after 3 hours under 40 ℃ of conditions; Be warming up to 70 ℃; Adding the 50kg insulation again soaked 2 hours; Filter liquide adds 50kg water insulation 1 hour again; Filter the hollow cellulose ultra-filtration membrane ultrafiltration of extracting solution adding molecular weight cut-off 5000; The hollow cellulose nanofiltration membrane that adds molecular weight cut-off 200 through liquid again concentrates; Get concentrated solution, add equal-volume 95% ethanolic soln and filter, add the equal-volume ethyl acetate extraction again 1 time; Raffinate adds 80g gac reflux decolour; Destainer filters and is concentrated into no pure crystallization, and crystallisate leaches the dry ecdysterone 78g of getting, content 85%.
Embodiment 3:
The amaranthaceous plant Root of Willowleaf Achyranthes is pulverized; Get 10kg and add extractor; Taking by weighing the 10g polygalacturonase is dissolved in the aqueous solution of 10kgph5 and adds extractor; Enzymolysis is after 3 hours under 50 ℃ of conditions; Be warming up to 70 ℃; Adding the 50kg insulation again soaked 1 hour; Filter liquide adds 50kg water insulation 1 hour again; Filter the hollow cellulose ultra-filtration membrane ultrafiltration of extracting solution adding molecular weight cut-off 3000; The hollow cellulose nanofiltration membrane that adds molecular weight cut-off 300 through liquid again concentrates; Get concentrated solution, add equal-volume 95% ethanolic soln and filter, add 1/2 volumes of acetic acid ethyl ester extraction 2 times again; Raffinate adds 60g gac reflux decolour; Destainer filters and is concentrated into no pure crystallization, and crystallisate leaches the dry ecdysterone 55g of getting, content 81%.
Claims (4)
1. method of from plant, extracting ecdysterone is characterized in that following steps:
A. raw material pulverizing adds biological enzyme after under the 40-50 ℃ of condition enzymolysis 2-3 hour, adds water and is warming up to 70-80 ℃, and insulation was soaked 1-2 hour, extracted 2-3 time, crosses and filters extracting solution;
B. said extracted liquid adds the ultra-filtration membrane ultrafiltration, adds nanofiltration membrane again through liquid and concentrates, and concentrated solution adds the equal-volume ethanolic soln and filters; Add ethyl acetate extraction again; Raffinate adds the gac reflux decolour, and destainer filters and is concentrated into no pure crystallization, the dry ecdysterone that gets of crystallisate.
2. from plant, extract the method for ecdysterone according to claim 1, it is characterized in that the optional Commelianaceae tabasheer of raw material Radix Cyanotis vagae, labiate japanese bugle herb and amaranthaceous plant Root of Willowleaf Achyranthes among the described step a.
3. from plant, extract the method for ecdysterone according to claim 1, it is characterized in that the biological enzyme among the described step a is a kind of or arbitrary combination in cellulase, amylase and the polygalacturonase, consumption is the 1-3 ‰ of material quantity.
4. from plant, extract the method for ecdysterone according to claim 1; It is characterized in that the ultra-filtration membrane among the described step b is the hollow cellulose ultra-filtration membrane of molecular weight cut-off 2000-5000, nanofiltration membrane is the hollow cellulose nanofiltration membrane of molecular weight cut-off 100-300.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110264182XA CN102351936A (en) | 2011-09-08 | 2011-09-08 | Method for extracting ecdysterone from plant |
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| CN201110264182XA CN102351936A (en) | 2011-09-08 | 2011-09-08 | Method for extracting ecdysterone from plant |
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| CN102351936A true CN102351936A (en) | 2012-02-15 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102872167A (en) * | 2012-09-29 | 2013-01-16 | 楚雄州百草岭药业发展有限公司 | Cyanotis root extract rich in beta-ecdysone and preparation method thereof |
| CN106176554A (en) * | 2016-08-31 | 2016-12-07 | 童风 | A kind of spot-removing ointment |
| CN108084242A (en) * | 2017-12-28 | 2018-05-29 | 云南汉德生物技术有限公司 | A kind of method for extracting moulting hormone |
| CN111493217A (en) * | 2019-08-16 | 2020-08-07 | 佛山市信豚生物科技有限公司 | Compound premix for promoting exuviation of shrimps and crabs as well as preparation method and feed thereof |
| CN112394121A (en) * | 2020-12-25 | 2021-02-23 | 成都普思生物科技股份有限公司 | Method for determining content of synechocystin B in achyranthes bidentata |
| CN112724190A (en) * | 2021-01-12 | 2021-04-30 | 四川兴杰象药业有限公司 | Method for extracting ecdysone from herba Eragrostis Nigrae |
| CN112851737A (en) * | 2021-01-12 | 2021-05-28 | 四川兴杰象药业有限公司 | System and method for efficiently extracting ecdysone |
-
2011
- 2011-09-08 CN CN201110264182XA patent/CN102351936A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102872167A (en) * | 2012-09-29 | 2013-01-16 | 楚雄州百草岭药业发展有限公司 | Cyanotis root extract rich in beta-ecdysone and preparation method thereof |
| CN102872167B (en) * | 2012-09-29 | 2014-11-12 | 楚雄州百草岭药业发展有限公司 | Cyanotis root extract rich in beta-ecdysone and preparation method thereof |
| CN106176554A (en) * | 2016-08-31 | 2016-12-07 | 童风 | A kind of spot-removing ointment |
| CN108084242A (en) * | 2017-12-28 | 2018-05-29 | 云南汉德生物技术有限公司 | A kind of method for extracting moulting hormone |
| CN111493217A (en) * | 2019-08-16 | 2020-08-07 | 佛山市信豚生物科技有限公司 | Compound premix for promoting exuviation of shrimps and crabs as well as preparation method and feed thereof |
| CN112394121A (en) * | 2020-12-25 | 2021-02-23 | 成都普思生物科技股份有限公司 | Method for determining content of synechocystin B in achyranthes bidentata |
| CN112724190A (en) * | 2021-01-12 | 2021-04-30 | 四川兴杰象药业有限公司 | Method for extracting ecdysone from herba Eragrostis Nigrae |
| CN112851737A (en) * | 2021-01-12 | 2021-05-28 | 四川兴杰象药业有限公司 | System and method for efficiently extracting ecdysone |
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Application publication date: 20120215 |