CN103664842A - Continuous chromatographic separation method for andrographolide - Google Patents
Continuous chromatographic separation method for andrographolide Download PDFInfo
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- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/56—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
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Abstract
The invention relates to a continuous chromatographic separation method for andrographolide. With the adoption of the method, andrographolide is efficiently extracted and separated through a continuous chromatographic separation process; and firstly, leaves of andrographis paniculata are extracted by ethyl alcohol, then, a part of ethyl alcohol is recycled and concentrated, and a column liquid is obtained; the column liquid absorbs andrographolide through a continuous chromatographic system, and an andrographolide crude product is obtained after elution by eluent, concentration and crystallization; and an andrographolide fine product is obtained after recrystallization.
Description
Technical field
The present invention relates to the separation method of rographolide, described method is utilized disk delivering continuous chromatography separated rographolide from Herba Andrographis extracting solution thing.
Background technology
Herba Andrographis Androgrophis paniculata (Bum.F.) Nees is Acanthaceae Herba Andrographis platymiscium, originates in subtropical zone, and cultivate more in the warm area on the south China the Changjiang river.Medicinal leaf or herb, at the beginning of the autumn, cauline leaf flower is tapped, and dries.There is clearing heat and detoxicating, swelling and pain relieving effect, by < < Chinese Pharmacopoeia > >, recorded.Rographolide be Chinese medicine Herba Andrographis mainly contain one of effective constituent, there is antipyretic, anti-inflammatory, antiviral, hepatic cholagogic, the effect such as hypoglycemic, main by treatment infantile pneumonia clinically, upper respiratory tract infection, and there is significant effect at aspects such as immunomodulatory, antitumor, anti-diabetics.Research shows that rographolide and dehydration Herba Andrographis ester have significant HIV (human immunodeficiency virus)-resistant activity, and EC50 is respectively 49.0 and 56.8ug/ml, but all well below the activity (EC50 is 20ng/ml) of inverase AZT.Along with to the deepening continuously of rographolide and derivative pharmacology activity research thereof, further prove that rographolide and derivative thereof have pharmacologically active widely, and shown the application prospect of wide deep exploitation.The traditional Chinese medicine Xiyanping that the sulfonated bodies of rographolide is made, in the great communicable disease for the treatment of (H1N1 first stream, hand foot mouth disease etc.), has been obtained good curative effect, and year sales volume is over 1,000,000,000 yuan.
Chinese patent CN1935798B discloses a kind of preparation method of rographolide, is divided into following four steps:
Step 1 is: get Herba Andrographis 400g, be ground into meal or section, add 8 times of amount 75-85% alcohol reflux 2 times, each 1 hour; Filter, merging filtrate, lets cool, standby;
Step 2 is: AB-8 type macroporous resin on extracting solution, and flow velocity 2-2.5BV/h, collects filtrate, and 70 ℃ are evaporated to determining alcohol is below 20-28%, filters, and with concentration ethanol washing precipitation, washings and filtrate are mixed to volume and are 400ml, standby;
Step 3 is: get filtrate, upper AB-8 type macroporous resin flow velocity 1-1.5BV/h, with 4 times of column volume 30% alcohol flushings, then uses 6 times of amounts of 35-40% ethanol, and wash-out is collected elutriant;
Step 4 is: in elutriant, add 200-300 order silica gel 8g, 70 ℃ be evaporated to below dry, washing with acetone 3 times, each 100ml, ultrasonic dissolution, filters, merging filtrate, and 60 ℃ are evaporated to dry below, washing with acetone precipitation 3-4 time, 5-10ml/ time, precipitation is dry.
The separated rographolide of this patented method need repeat upper prop, and suitability for industrialized production more complicated, is unfavorable for scale operation.Because rographolide and the rographolide polarity of anhydrating differ less, while causing rographolide separated with deoxydidehydrorographolide, have and intersects and make yield reduction.This is purified and mainly adopts fixed bed partition method simultaneously.The rographolide that this traditional separation method separation obtains exists that purity is low, eluent consumption is large, the cycle is long, environmental protection pressure is large, the not high shortcomings of resin utilization ratio.Therefore need to develop efficient process for separating and purifying, to improve the quality of products, advocate Green Chemistry.
Summary of the invention
The present invention utilizes continuous chromatography to carry out separation to rographolide, makes rographolide can obtain better separation.
The structural formula of rographolide is as follows:
Continuous chromatography separation method of the present invention is separated rographolide from Herba Andrographis ethanol extraction, described method, and step is as follows:
A. Herba Andrographis ethanol extract is concentrated into finite concentration, the centrifugal precipitation of removing.
B. by the upper continuous chromatography post of filtrate, obtain the elutriant that contains rographolide, the concentrated concentrated solution that to obtain of elutriant;
C. concentrated solution adds 1% activated carbon, silica gel or the decolouring of silicon bath soil, filters, and obtains destainer, and the alcohol concn in adjusting destainer, to 25-30%, is placed crystallization, collects crystallization and obtains rographolide crude product.
D. get crude product and add 15 times of (V/W) ethanol, reflux makes to dissolve, and proper amount of active carbon or diatomite decolouring (20-30% of crude product weight), filter, and places crystallization, collects crystallization and obtains rographolide.
Wherein, Herba Andrographis ethanol extract described in step a, is the extracting solution that Herba Andrographis medicinal material is obtained with extraction using alcohol, belongs to prior art, can obtain according to art methods, as the method for Chinese patent CN1935798B.
Continuous chromatography post described in step b, the chromatographic column of employing is 20-30 root, and with macroporous adsorbent resin, as filler, its model is HPD-100 or DA-201 type, and resin aperture is 30-80 order, and the chromatographic column in each district adopts respectively serial or parallel connection mode to connect; 20% washing with alcohol for Xi Za district, resolves district and resolves with the ethanol of 30-55%, 95% ethanol activating and regenerating for breeding blanket.
The preferred disk delivering of the present invention continuous chromatography separation system, this system is divided into adsorption zone, Xi Za district, resolves district, Si Ge district, regeneration washing district.
1) adsorption zone: this district has 3～8 unit, by flow rate control, first raw material enters chromatographic column group in parallel, then by all the other pole units of series connection, the effluent liquid of No. 1 mouth is waste liquid, enters three wastes center processing.
2) Xi Za district (1 unit): after absorption, the ethanol of each resin container needs 20% is washed, and is positioned at behind adsorption zone.Resin container forwards to behind absorption water wash zone, is entrained in the feed liquid (be mainly clear liquor) of tree between referring to and is ejected by water, and the effluent liquid mixing of No. 1 mouth of effluent liquid and adsorption zone together enters 4(9) resin container that number unit is corresponding.Wash away and be clipped in the feed liquid of resin gap and take away impurity as far as possible, preventing that feed liquid from carrying secretly resolves district, improve the purity of desorbed solution, and its ethanol of 20% is incorporated to adsorption zone, effective constituent in planar water washing lotion again, by getting 4(9) number outlet sample after TLC detects to determine washing effect.
3) resolve district (12～22 unit): at this, resolve district, with continuous, gradient analysis mode, resolve district and all take positive charging, collect and respectively export desorbed solution respectively, according to processing method, design is divided into following several part: 35～45% ethanol, desorbed solution is collected, mainly containing rographolide; 55% ethanol, desorbed solution is collected and is mainly deoxydidehydrorographolide;
4) regeneration washing district (4～8 unit): all separately chargings, and be suitable, backward feed, thus the ethanol recovery of the flushing 95% after each step regeneration is adjusted alcohol concn again and is reached recycling.Refer to Figure of description.
The rographolide that the inventive method separation obtains, its very high purity.Its method for detecting purity is pressed < < Chinese Pharmacopoeia > > 2010 editions.Use Agilent 1260 high performance liquid chromatographs.Chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as weighting agent; The methanol-water (60:40) of take is moving phase; Detection wavelength is 225nm.Number of theoretical plate calculates and is not less than 5000 by rographolide peak.Three BT(batch testing) results are as follows:
| Batch | 1 | 2 | 3 |
| Rographolide purity (%) | 99.2 | 100.3 | 99.5 |
Continuous chromatography separation method of the present invention, and existing bed technology comparison, the comparative data of beneficial effect is as follows:
The present invention has improved original fixed bed separating device, make the absorption of original fixed bed, wash assorted, wash-out, the whole workshop sections such as regeneration are incorporated in disk delivering adverse current continuous chromatography separation system, it is divided into some sections by whole section of resin in original fixed bed, part resin before former processing method tradition district is positioned at one or several little resin column again, so just can reenter absorption, wash-out, regeneration waits in circulation, utilized the part resin of originally not reinstated, resin utilization ratio has just improved greatly, can also reduce chemical reagent simultaneously, the consumption of water etc.Disk delivering continuous chromatography separation system has a large amount of post (separation) unit, also makes them can very effectively be applied to series classification production process.According to the characteristic of each composition in rographolide, the selected resin of the present invention is macroporous adsorbent resin, and resin particle diameter is at 30～80 orders, and uniformity coefficient is more than 95%.
Use above-mentioned continuous chromatography separation system, compared to the prior art superiority is:
Benefit of the present invention: 1) institute of fixed-bed process is all integrated in a set of process system in steps, is that system is simplified, and reduces the layout of process pipe, system compact, can realize automatization and control; Floor space saves 80%, and factory building height only needs 1/3 of fixed bed height, and the investment in fixed assets of same throughput is saved more than 30%.2) resin utilization ratio is high, is product concentration, purity and yield optimization; Technique of the present invention and the comparison of fixed-bed resin separating technology, its resin demand is only original 30%, and can be than being easier to carry out forward and inverse stream in resin inside, the resin that can loosen, prevents its caking.3) reduce the consumption of chemical reagent and water, reduce the discharge of waste water; Utilize this technique to return cover to material and use, reach recycle.4) system adopts self-con-tained unit, reduces work load.5) enhance productivity, improve production capacity, the production cycle has reduced by 1/3 time with respect to former fixed-bed resin separating technology.
Accompanying drawing explanation
Fig. 1 is equipment and process schema.
Embodiment
Embodiment 1:
Get 10 kilograms of Folium Andrographis, with the ethanol of 3 times of amount (in charging capacitys) 80%, infiltrate, 80% the ethanol percolation by 10 times of amounts (in charging capacity), reclaims ethanol to containing ethanol content approximately 40%, centrifugal, removal chlorophyll.
Select HPD100 type macroporous adsorbent resin, resin is 30～80 orders, and each resin column amount of fill is 0.005m
3, resin column is of a size of Ф 10 * 60mm, and actual filling ratio is 80% left and right.
The separated rographolide of disk delivering continuous chromatography separation system divides following region:
1) adsorption zone: (Unit 1～6)
This region has 6 unit (1,2,3,4,5 and No. 6 chromatographic column), and by flow rate control, first raw material enters the chromatographic column group by 5 and No. 6 chromatographic column parallel connections, then by all the other pole units of series connection, the effluent liquid of No. 1 mouth is waste liquid, enters three wastes center processing.
2) Xi Za district: (Unit 7)
After absorption, the ethanol of each resin needs 20% is washed, and is positioned at behind adsorption zone.Resin column rotates to absorption 20% ethanol and washes behind district, being entrained in feed liquid (being mainly clear liquor) between the macroporous resin ethanol by 20% ejects, wash away and be mixed in the feed liquid of resin gap and take away impurity as far as possible, preventing that feed liquid from carrying secretly to enter resolves district, improve the purity of stripping liquid, and its ethanol washing lotion of 20% is entered into adsorption zone, the active principle in planar water washing lotion again, by No. 7 outlet samples after TLC detects to determine washing effect.
3) resolve district
At this, resolve district, with continuous, gradient analysis mode, resolve district and all take positive charging, collect and respectively export desorbed solution respectively, according to processing method, design is divided into following a few part:
1) connect for 8～No. 13 into 30% ethanol, stripping liquid directly enters water drain;
2) connect for 14～No. 21 into 35% ethanol, desorbed solution is collected and is mainly rographolide;
3) connect for 21～No. 24 into 55% ethanol, desorbed solution is collected and is mainly the impurity such as deoxydidehydrorographolide;
4) regeneration washing district (25～No. 30 unit);
Unit, 6, this district is charging separately all, and is reverse or forward feed, with 95% ethanol, regenerates.
Separation purity: resolve product and divide three parts.Collect the requirement that part can meet downstream process 14～No. 21; Rographolide separates completely with other components.The lap of rographolide and other components is by directly getting back to material mouthful after regulating, as a part for feeding liquid.
In this continuous chromatography separation system, can accomplish batch interior reuse, the ethanol eluate of 20% after absorption can come back to adsorption zone, and the loss while so just reducing absorption, fully exchanges the active principle in feed liquid; The ethanol of adsorption zone, Xi Za district, desorption zone and breeding blanket is all recyclable, regulates concentration as washing assorted or resolving and use.
The stripping liquid containing rographolide of collecting is adjusted to alcohol concn to 25～30%, place a few hours, when starting crystallization, stir gently crystal, can obtain the rographolide crude product that crystalline form is consistent.Get crude product and add 15 times of (V/W) ethanol, reflux makes to dissolve, and proper amount of active carbon (20-30% of crude product weight) is filtered, and places crystallization and get final product.
Embodiment 2:
Get 10 kilograms of Folium Andrographis, with the ethanol of 3 times of amount (in charging capacitys) 90%, infiltrate, 90% the ethanol percolation by 10 times of amounts (in charging capacity), reclaims ethanol to containing ethanol content approximately 40%, centrifugal, removal chlorophyll.Select DA201 type macroporous adsorbent resin, resin is 30～80 orders, and each resin column amount of fill is 0.005m
3, resin column is of a size of Ф 10 * 60mm, and actual filling ratio is 80% left and right.
The separated rographolide of disk delivering continuous chromatography separation system divides following region:
1) adsorption zone: (1～unit 8)
This region has 8 unit (1,2,3,4,5,6,7 and No. 8 chromatographic column), by flow rate control, first raw material enters the chromatographic column group by 6,7, No. 8 chromatographic column parallel connections, then by all the other pole units of series connection, the effluent liquid of No. 1 mouth is waste liquid, enters three wastes center processing.
2) Xi Za district: (Unit 9)
After absorption, the ethanol of each resin needs 20% is washed, and is positioned at behind adsorption zone.Resin column rotates to absorption 20% ethanol and washes behind district, being entrained in feed liquid (being mainly clear liquor) between the macroporous resin ethanol by 20% ejects, wash away and be mixed in the feed liquid of resin gap and take away impurity as far as possible, preventing that feed liquid from carrying secretly to enter resolves district, improve the purity of stripping liquid, and its ethanol washing lotion of 20% is entered into adsorption zone, the active principle in planar water washing lotion again, by No. 9 outlet samples after TLC detects to determine washing effect.
3) resolve district
At this, resolve district, with continuous, gradient analysis mode, resolve district and all take positive charging, collect and respectively export desorbed solution respectively, according to processing method, design is divided into following a few part:
1) connect for 10～No. 15 into 35% ethanol, stripping liquid directly enters water drain;
2) connect for 16～No. 23 into 45% ethanol, desorbed solution is collected and is mainly rographolide;
3) connect for 24～No. 26 into 55% ethanol, desorbed solution is collected and is mainly the impurity such as deoxydidehydrorographolide;
4) regeneration washing district (27～No. 30 unit);
Unit, 4, this district is charging separately all, and is reverse or forward feed, with 95% ethanol, regenerates.
Separation purity: resolve product and divide three parts.Collect the requirement that part can meet downstream process 16～No. 23; Rographolide separates completely with other components.The lap of rographolide and other components is by directly getting back to material mouthful after regulating, as a part for feeding liquid.
In this continuous chromatography separation system, can accomplish batch interior reuse, the ethanol eluate of 20% after absorption can come back to adsorption zone, and the loss while so just reducing absorption, fully exchanges the active principle in feed liquid; The ethanol of adsorption zone, Xi Za district, desorption zone and breeding blanket is all recyclable, measures concentration as washing assorted or resolving and use.
The stripping liquid containing rographolide of collecting is adjusted to alcohol concn to 25～30%, place a few hours, when starting crystallization, stir gently crystal, can obtain the rographolide crude product that crystalline form is consistent.Get crude product and add 15 times of (V/W) ethanol, reflux makes to dissolve, and appropriate diatomite (20-30% of crude product weight), filters, and places crystallization and get final product.
Claims (1)
1. a continuous chromatography separation method for rographolide, comprises the following steps:
A) get Herba Andrographis medicinal material, be ground into meal, add 80～90% alcohol dipping, the ethanol percolation with 80～90%, collects the percolate of 6～10 times of amounts, and decompression recycling ethanol is to containing alcohol amount 40%, and the centrifugal chlorophyll of removing precipitates.
B) get HPD100 type or DA201 type macroporous resin continuous chromatography post on supernatant liquor.First use 20% ethanol removal of impurities, respectively with the ethanol elution of 35～45% ethanol and 50～55%.
C) by 35～45% ethanol eluates with concentrating.Concentrated solution adds 1% decolorizing with activated carbon, filters, and gets destainer.Regulate alcohol concn to 25～30%, place a few hours, when starting crystallization, stir gently crystal, can obtain the rographolide crude product that crystalline form is consistent.
D) get crude product and add 15 times of (V/W) ethanol, reflux makes to dissolve, and proper amount of active carbon or diatomite decolouring (20-30% of crude product weight), filter, and places crystallization and get final product.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104447642A (en) * | 2014-12-19 | 2015-03-25 | 黄曦 | Chromatographic separation and purification method for industrially preparing andrographolide |
| CN104557818A (en) * | 2014-12-16 | 2015-04-29 | 浙江维康药业有限公司 | Common andrographis herb lactone compound as well as dropping pills and soft capsules containing compound |
| CN104557820A (en) * | 2014-12-19 | 2015-04-29 | 浙江大学 | Method for purifying andrographolide |
| CN110194753A (en) * | 2019-07-15 | 2019-09-03 | 成都通德药业有限公司 | A kind of andrographolide process for refining |
| CN112979594A (en) * | 2021-02-26 | 2021-06-18 | 南通科鑫超临界设备有限公司 | Supercritical extraction process of andrographolide |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104557818A (en) * | 2014-12-16 | 2015-04-29 | 浙江维康药业有限公司 | Common andrographis herb lactone compound as well as dropping pills and soft capsules containing compound |
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| CN104557820A (en) * | 2014-12-19 | 2015-04-29 | 浙江大学 | Method for purifying andrographolide |
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| CN110194753A (en) * | 2019-07-15 | 2019-09-03 | 成都通德药业有限公司 | A kind of andrographolide process for refining |
| CN112979594A (en) * | 2021-02-26 | 2021-06-18 | 南通科鑫超临界设备有限公司 | Supercritical extraction process of andrographolide |
| CN112979594B (en) * | 2021-02-26 | 2021-12-14 | 南通科鑫超临界设备有限公司 | Supercritical extraction process of andrographolide |
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Application publication date: 20140326 |