CN103421016A - Anthricin preparation method - Google Patents
Anthricin preparation method Download PDFInfo
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- CN103421016A CN103421016A CN2013103601104A CN201310360110A CN103421016A CN 103421016 A CN103421016 A CN 103421016A CN 2013103601104 A CN2013103601104 A CN 2013103601104A CN 201310360110 A CN201310360110 A CN 201310360110A CN 103421016 A CN103421016 A CN 103421016A
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Abstract
The invention discloses an anthricin preparation method. The method includes the following steps: 1), taking anthricin for smashing, adding 5-10 times of amount of 30-90% ethanol solution, performing reflux extraction for 2-3 times, concentrating an extracting solution to be alcohol-free, adding the extraction solution in macroporous resin for adsorption, using ethanol solution for gradient elution, collecting eluent, depressurizing for concentration, adding benzene solution in size volume and fully stirring, collecting a benzene solution layer to be concentrated to a small size, and placing for crystallization; 2), dissolving obtained crystals by 5-10 times of amount of 80-90% methanol, adding activated carbon for decoloring, concentrating filtrate to enable alcohol concentration to be 30-50%, extracting by benzene solution, adding 1/3-1/10 ethanol solution in extract liquor, placing for recrystallizing, and drying crystal substances to obtain anthricin. The anthricin preparation method is simple and convenient in process operation, low in production cost and easy to realize industrial production.
Description
Technical field
The invention belongs to the biotechnology chemical field, particularly a kind of preparation method of anthricin.
Background technology
Anthricin is the lignin material, CAS 24150-39-8, molecule is C22H22O7, molecular weight 398.4, colourless column crystallization, fusing point 166-169, have protect the liver, antiviral, antitumor action.
The root that wild chervil is the samphire wild chervil, invigorating the spleen and replenishing QI, promoting tissue regeneration by removing blood stasis.Root: for wound, pain in the back, cough due to deficiency of the lung, cough spitting of blood, splenasthenic abdominal distention, myasthenia of the limbs, old man's frequent micturition, oedema; Leaf: wound is controlled in external application.Modern study is found to contain a large amount of lignin materials in wild chervil, as anthricin, isoanthricin etc.,
By literature search, existing anthricin preparation method adopts the silica gel separation method is arranged.Due to complicated operation, preparation amount is less, and the sample yield is low, is difficult to realize suitability for industrialized production.
Summary of the invention
The objective of the invention is to solve shortcomings and deficiencies of the prior art, a kind of preparation method of anthricin easy and simple to handle is provided.
To achieve these goals, the present invention is by the following technical solutions: a kind of preparation method of anthricin is characterized in that following steps:
1) getting wild chervil pulverizes, add 5-10 doubly to measure the 30%-90% ethanolic soln, refluxing extraction 2-3 time, extracting solution is reduced to without alcohol and adds in macroporous resin and adsorb, the ethanolic soln gradient elution, collect elutriant, concentrating under reduced pressure, add the equal-volume benzole soln fully to stir, collect the benzole soln layer and be concentrated into small volume placement crystallization;
2) the gained crystallization is doubly measured the 80%-90% dissolve with methanol with 5-10, adds activated carbon decolorizing, and filtrate is concentrated into determining alcohol 30%-50% again with the benzole soln extraction, and extraction liquid adds the 1/3-1/10 ethanolic soln to place recrystallization, and crystallisate is drying to obtain.
A kind of in the optional AB-8 of macroporous resin described in step 1), D101, HZ816, HPD100.
Ethanolic soln gradient elution described in step 1) for first with 5-10 times of column volume 20%-50% ethanol elution, then with 5-10 times of column volume 70%-90% ethanolic soln wash-out.
Adopt this law to produce anthricin, simple process is easy to operate, and product purity is high, is easy to realize preparation of industrialization.
Further illustrate the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment
Embodiment 1:
Getting the 10kg wild chervil pulverizes, add 5 times of amount 70% ethanolic solns, refluxing extraction 3 times, united extraction liquid is reduced to without alcohol and adds in the AB-8 macroporous resin and adsorb, and first uses 8 times of column volume 30% ethanol elutions, then uses 7 times of column volumes, 75% ethanolic soln wash-out, collect elutriant, concentrating under reduced pressure, add the equal-volume benzole soln fully to stir in concentrated solution, collect the benzole soln layer and be concentrated into small volume placement crystallization.10 times of amount 80% dissolve with methanol for the gained crystallization, add activated carbon decolorizing, and filtrate is concentrated into determining alcohol 30% again with benzole soln extraction 2 times, and extraction liquid adds 1/3 ethanolic soln to place recrystallization, and crystallisate obtains anthricin 3.5g, detects content 98.6% through HPLC.
Embodiment 2:
Getting the 10kg wild chervil pulverizes, add 10 times of amount 30% ethanolic solns, refluxing extraction 2 times, united extraction liquid is reduced to without alcohol and adds in the D101 macroporous resin and adsorb, and first uses 5 times of column volume 20% ethanol elutions, then uses 10 times of column volumes, 70% ethanolic soln wash-out, collect elutriant, concentrating under reduced pressure, add the equal-volume benzole soln fully to stir in concentrated solution, collect the benzole soln layer and be concentrated into small volume placement crystallization.5 times of amount 90% dissolve with methanol for the gained crystallization, add activated carbon decolorizing, and filtrate is concentrated into determining alcohol 50% again with benzole soln extraction 2 times, and extraction liquid adds 1/10 ethanolic soln to place recrystallization, and crystallisate obtains anthricin 3.1g, detects content 97.4% through HPLC.
Embodiment 3:
Getting the 10kg wild chervil pulverizes, add 10 times of amount 90% ethanolic solns, refluxing extraction 2 times, united extraction liquid is reduced to add after suitable quantity of water solution to add in the HZ816 macroporous resin without alcohol again and adsorbs, and first uses 5 times of column volume 50% ethanol elutions, then uses 10 times of column volumes, 75% ethanolic soln wash-out, collect elutriant, concentrating under reduced pressure, add the equal-volume benzole soln fully to stir in concentrated solution, collect the benzole soln layer and be concentrated into small volume placement crystallization.8 times of amount 80% dissolve with methanol for the gained crystallization, add activated carbon decolorizing, and filtrate is concentrated into determining alcohol 40% again with benzole soln extraction 2 times, and extraction liquid adds 1/5 ethanolic soln to place recrystallization, and crystallisate obtains anthricin 3.9g, detects content 98.1% through HPLC.
Embodiment 4:
Getting the 10kg wild chervil pulverizes, add 10 times of amount 70% ethanolic solns, refluxing extraction 2 times, united extraction liquid is reduced to add after suitable quantity of water solution to add in the HPD100 macroporous resin without alcohol again and adsorbs, and first uses 5 times of column volume 40% ethanol elutions, then uses 10 times of column volumes, 70% ethanolic soln wash-out, collect elutriant, concentrating under reduced pressure, add the equal-volume benzole soln fully to stir in concentrated solution, collect the benzole soln layer and be concentrated into small volume placement crystallization.10 times of amount 90% dissolve with methanol for the gained crystallization, add activated carbon decolorizing, and filtrate is concentrated into determining alcohol 30% again with benzole soln extraction 2 times, and extraction liquid adds 1/3 ethanolic soln to place recrystallization, and crystallisate obtains anthricin 3.3g, detects content 97.3% through HPLC.
Claims (3)
1. the preparation method of an anthricin is characterized in that following steps:
1) getting wild chervil pulverizes, add 5-10 doubly to measure the 30%-90% ethanolic soln, refluxing extraction 2-3 time, extracting solution is reduced to without alcohol and adds in macroporous resin and adsorb, the ethanolic soln gradient elution, collect elutriant, concentrating under reduced pressure, add the equal-volume benzole soln fully to stir, collect the benzole soln layer and be concentrated into small volume placement crystallization;
2) the gained crystallization is doubly measured the 80%-90% dissolve with methanol with 5-10, adds activated carbon decolorizing, and filtrate is concentrated into determining alcohol 30%-50% again with the benzole soln extraction, and extraction liquid adds the 1/3-1/10 ethanolic soln to place recrystallization, and crystallisate is drying to obtain.
2. the preparation method of thorn anthricin according to claim 1, is characterized in that a kind of in the optional AB-8 of the macroporous resin described in step 1), D101, HZ816, HPD100.
3. the preparation method of anthricin according to claim 1, it is characterized in that the ethanolic soln gradient elution described in step 1) for first with 5-10 times of column volume 20%-50% ethanol elution, then with 5-10 times of column volume 70%-90% ethanolic soln wash-out.
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| CN2013103601104A CN103421016A (en) | 2013-08-19 | 2013-08-19 | Anthricin preparation method |
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| CN2013103601104A CN103421016A (en) | 2013-08-19 | 2013-08-19 | Anthricin preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103965209A (en) * | 2014-05-15 | 2014-08-06 | 中国药科大学 | Novel crystal forms for deoxypodophyllotoxin and preparation method of novel crystal forms |
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2013
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103965209A (en) * | 2014-05-15 | 2014-08-06 | 中国药科大学 | Novel crystal forms for deoxypodophyllotoxin and preparation method of novel crystal forms |
| CN105017274A (en) * | 2014-05-15 | 2015-11-04 | 中国药科大学 | Novel crystal forms of deoxypodophyllotoxin and preparation methods thereof |
| CN105017274B (en) * | 2014-05-15 | 2017-01-18 | 中国药科大学 | Crystal forms of deoxypodophyllotoxin and preparation methods thereof |
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Application publication date: 20131204 |