CN105294618A - Method for extracting andrographolidume from Andrographis paniculata (Burm. F.) Nees - Google Patents
Method for extracting andrographolidume from Andrographis paniculata (Burm. F.) Nees Download PDFInfo
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- CN105294618A CN105294618A CN201510640943.5A CN201510640943A CN105294618A CN 105294618 A CN105294618 A CN 105294618A CN 201510640943 A CN201510640943 A CN 201510640943A CN 105294618 A CN105294618 A CN 105294618A
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- rographolide
- herba andrographis
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- mixed solvent
- chloroform
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- 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
- C07D307/60—Two oxygen atoms, e.g. succinic anhydride
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for extracting andrographolidume from Andrographis paniculata (Burm. F.) Nees. The method is characterized by comprising the following steps: 1) extracting the Andrographis paniculata (Burm. F.) Nees by 75 to 95v% ethyl alcohol, filtering an extracting solution, and taking filtrate for standby; 2) adding activated carbon into the filtrate to carry out decoloration, and filtering to obtain supernatant liquid; 3) after the supernatant liquid is concentrated, putting a silica gel column to carry out chromatography, washing the column with water until the column is colorless, then, carrying out elution by a mixed solvent of normal hexane and chloroform, and collecting a mixed solvent eluent; 4) carrying out solvent recovery on the eluent, and drying to obtain the andrographolidume. The mixed solvent of the normal hexane and the chloroform is adopted as the eluent, users can surprisedly find that the andrographolidume can be favorably eluted, finished product purity is high, and yield is high.
Description
Technical field
The invention belongs to active components of plants extractive technique field, relate generally to a kind of method extracting rographolide from Herba Andrographis.
Background technology
Herba Andrographis is the dry aerial parts of acanthaceous plant Herba Andrographis (Andrographispaniculata (Burm.F.) Nees), has the functions such as clearing heat and detoxicating, cool blood detumescence.Herba Andrographis main active ingredient is rographolide, is the principle active component of the conventional Chinese patent medicine creat formulations such as treatment upper respiratory tract infection, acute bacillary dysentery, viral cold.Existing rographolide extracting and purifying method is a lot, and first by Herba Andrographis alcohol extracting, with petroleum ether extraction, then cross macroporous resin, carry out wash-out with the ethanol of different concns, the rographolide purity finally obtained is not high, and yield is lower.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method extracting rographolide from Herba Andrographis, and the rographolide purity that the method obtains is high, and yield is large.
Technical scheme provided by the invention is a kind of method extracting rographolide from Herba Andrographis, comprises the following steps:
1) get Herba Andrographis 75 ~ 95v% extraction using alcohol, by extracting liquid filtering, it is for subsequent use to get filtrate;
2) in filtrate, add activated carbon decolorizing, filter, obtain clear liquor;
3) after clear liquor is concentrated, upper silica gel column chromatography, washing post, to colourless, then carries out wash-out with the mixed solvent of normal hexane and chloroform, collects mixed solvent elutriant;
4) by elutriant recycling design, dry, be rographolide.
Step 1) in, the consumption of ethanol is 10 ~ 30 times of Herba Andrographis weight, and at 40 ~ 60 DEG C, refluxing extraction 1 ~ 3 time, extracts 1 ~ 3h at every turn.
Step 2) in, the add-on of gac is 1 ~ 1.5 ‰ of filtrate gross weight, and bleaching temperature is 40 ~ 60 DEG C, and bleaching time is 20 ~ 30min.
Step 3) in, the volume ratio of normal hexane and chloroform is 50 ~ 80:20 ~ 50.As preferably, the volume ratio of normal hexane and chloroform is 80:20, now can maximum wash-out rographolide, and yield is large, and purity is high.
Step 3) in, during upper prop, the flow velocity of concentrated solution is 0.5 ~ 1BV/h; During wash-out, the flow velocity of water is 0.5 ~ 1BV/h, and consumption is 1 ~ 2BV; The mobility of mixed solvent is 1 ~ 1.5BV/h, and consumption is 2 ~ 2.5BV.
The present invention adopts the mixed solvent of normal hexane and chloroform as elutriant, and pleasantly surprised discovery energy wash-out rographolide preferably, finished product purity is high, and yield is large.After testing, product yield can reach more than 1.35%, high purity more than 96.8%.
Embodiment
The present invention is further elaborated for following specific embodiment, but not as a limitation of the invention.
Embodiment 1
1) get Herba Andrographis cured leaf 100g, use 75v% extraction using alcohol, the consumption of ethanol is 10 times of Herba Andrographis weight, refluxing extraction 1h at 40 DEG C, and by extracting liquid filtering, it is for subsequent use to get filtrate;
2) in filtrate, add activated carbon decolorizing, the add-on of gac is 1 ‰ of filtrate gross weight, and bleaching temperature is 40 DEG C, and bleaching time is 20min, filters, obtains clear liquor;
3) after clear liquor is concentrated, upper silica gel column chromatography, the flow velocity of concentrated solution is 0.5BV/h; Washing post is to colourless, and the flow velocity of water is 0.5BV/h, and consumption is 1BV; Then carry out wash-out with the mixed solvent of normal hexane and chloroform, the volume ratio of normal hexane and chloroform is 50:20, and the mobility of mixed solvent is 1BV/h, and consumption is 2BV, collects elutriant;
4) by elutriant recycling design, dry, weigh, obtain 1.35g rographolide.After testing, purity is 96.8%.
Embodiment 2
1) get Herba Andrographis cured leaf 100g, use 95v% extraction using alcohol, the consumption of ethanol is 30 times of Herba Andrographis weight, and at 60 DEG C, refluxing extraction 3 times, extracts 3h, united extraction liquid at every turn, filters, and it is for subsequent use to get filtrate;
2) in filtrate, add activated carbon decolorizing, the add-on of gac is 1.5 ‰ of filtrate gross weight, and bleaching temperature is 60 DEG C, and bleaching time is 30min, filters, obtains clear liquor;
3) after clear liquor is concentrated, upper silica gel column chromatography, the flow velocity of concentrated solution is 1BV/h; Washing post is to colourless, and the flow velocity of water is 1BV/h, and consumption is 2BV; Then carry out wash-out with the mixed solvent of normal hexane and chloroform, the volume ratio of normal hexane and chloroform is 80:50, and the mobility of mixed solvent is 1.5BV/h, and consumption is 2.5BV, collects elutriant;
4) by elutriant recycling design, dry, weigh, obtain 1.36g rographolide.After testing, purity is 96.8%.
Embodiment 3
1) get Herba Andrographis cured leaf 100g, use 80v% extraction using alcohol, the consumption of ethanol is 20 times of Herba Andrographis weight, and at 50 DEG C, refluxing extraction 2 times, extracts 2h, united extraction liquid at every turn, filters, and it is for subsequent use to get filtrate;
2) in filtrate, add activated carbon decolorizing, the add-on of gac is 1.5 ‰ of filtrate gross weight, and bleaching temperature is 60 DEG C, and bleaching time is 30min, filters, obtains clear liquor;
3) after clear liquor is concentrated, upper silica gel column chromatography, the flow velocity of concentrated solution is 1BV/h; Washing post is to colourless, and the flow velocity of water is 0.5 ~ 1BV/h, and consumption is 1 ~ 2BV; Then carry out wash-out with the mixed solvent of normal hexane and chloroform, the volume ratio of normal hexane and chloroform is 80:20, and the mobility of mixed solvent is 1.5BV/h, and consumption is 2.5BV, collects elutriant;
4) by elutriant recycling design, dry, weigh, obtain 1.45g rographolide.After testing, purity is 97.2%.
Embodiment 4
1) get Herba Andrographis cured leaf 100g, use 75v% extraction using alcohol, the consumption of ethanol is 30 times of Herba Andrographis weight, and at 40 DEG C, refluxing extraction 3 times, extracts 1h, united extraction liquid at every turn, filters, and it is for subsequent use to get filtrate;
2) in filtrate, add activated carbon decolorizing, the add-on of gac is 1 ‰ of filtrate gross weight, and bleaching temperature is 60 DEG C, and bleaching time is 20min, filters, obtains clear liquor;
3) after clear liquor is concentrated, upper silica gel column chromatography, the flow velocity of concentrated solution is 0.5BV/h; Washing post is to colourless, and the flow velocity of water is 1BV/h, and consumption is 1BV; Then carry out wash-out with the mixed solvent of normal hexane and chloroform, the volume ratio of normal hexane and chloroform is 80:20, and the mobility of mixed solvent is 1BV/h, and consumption is 2.5BV, collects elutriant;
4) by elutriant recycling design, dry, weigh, obtain 1.46g rographolide.After testing, purity is 97.3%.
Claims (6)
1. from Herba Andrographis, extract a method for rographolide, it is characterized in that: comprise the following steps:
1) get Herba Andrographis 75 ~ 95v% extraction using alcohol, by extracting liquid filtering, it is for subsequent use to get filtrate;
2) in filtrate, add activated carbon decolorizing, filter, obtain clear liquor;
3) after clear liquor is concentrated, upper silica gel column chromatography, washing post, to colourless, then carries out wash-out with the mixed solvent of normal hexane and chloroform, collects mixed solvent elutriant;
4) by elutriant recycling design, dry, be rographolide.
2. a kind of method extracting rographolide from Herba Andrographis according to claim 1, is characterized in that: step 1) in, the consumption of ethanol is 10 ~ 30 times of Herba Andrographis weight, and at 40 ~ 60 DEG C, refluxing extraction 1 ~ 3 time, extracts 1 ~ 3h at every turn.
3. a kind of method extracting rographolide from Herba Andrographis according to claim 1, is characterized in that: step 2) in, the add-on of gac is 1 ~ 1.5 ‰ of filtrate gross weight, and bleaching temperature is 40 ~ 60 DEG C, and bleaching time is 20 ~ 30min.
4. a kind of method extracting rographolide from Herba Andrographis according to claim 1, is characterized in that: step 3) in, the volume ratio of normal hexane and chloroform is 50 ~ 80:20 ~ 50.
5. a kind of method extracting rographolide from Herba Andrographis according to claim 4, is characterized in that: the volume ratio of normal hexane and chloroform is 80:20.
6. a kind of method extracting rographolide from Herba Andrographis according to claim 1, is characterized in that: step 3) in, during upper prop, the flow velocity of concentrated solution is 0.5 ~ 1BV/h; During wash-out, the flow velocity of water is 0.5 ~ 1BV/h, and consumption is 1 ~ 2BV; The mobility of mixed solvent is 1 ~ 1.5BV/h, and consumption is 2 ~ 2.5BV.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510640943.5A CN105294618A (en) | 2015-09-30 | 2015-09-30 | Method for extracting andrographolidume from Andrographis paniculata (Burm. F.) Nees |
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| CN201510640943.5A CN105294618A (en) | 2015-09-30 | 2015-09-30 | Method for extracting andrographolidume from Andrographis paniculata (Burm. F.) Nees |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106034622A (en) * | 2016-05-31 | 2016-10-26 | 山东胜伟园林科技有限公司 | Method of drip irrigation under plastic film through employing vitamin nutrient solution, and application of method in ryegrass planting in saline and alkaline lands |
| US11191798B2 (en) | 2016-11-02 | 2021-12-07 | Nutrition Science Partners Limited | Extracts of Andrographis paniculata, methods for preparation and use thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101559088A (en) * | 2009-05-21 | 2009-10-21 | 雷允上药业有限公司 | Production technique of andrographolide and neoandrographolide, dehydroanddrographolide, oxyandrographolide |
| US20120070519A1 (en) * | 2009-05-22 | 2012-03-22 | Bio-Ved Pharmaceuticals, Pvt. Ltd. | Method for extraction of fractions containing pharmacologically active ingredients with less cytotoxicity from one or more plants |
| CN102558257A (en) * | 2011-12-23 | 2012-07-11 | 柳州市绿翔生物技术有限公司 | Method for separating and purifying novel andrographolide |
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2015
- 2015-09-30 CN CN201510640943.5A patent/CN105294618A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101559088A (en) * | 2009-05-21 | 2009-10-21 | 雷允上药业有限公司 | Production technique of andrographolide and neoandrographolide, dehydroanddrographolide, oxyandrographolide |
| US20120070519A1 (en) * | 2009-05-22 | 2012-03-22 | Bio-Ved Pharmaceuticals, Pvt. Ltd. | Method for extraction of fractions containing pharmacologically active ingredients with less cytotoxicity from one or more plants |
| CN102558257A (en) * | 2011-12-23 | 2012-07-11 | 柳州市绿翔生物技术有限公司 | Method for separating and purifying novel andrographolide |
Non-Patent Citations (5)
| Title |
|---|
| SUDHANSHU SAXENA ET AL.: "High-Performance Thin-Layer Chromatographic Analysis of Hepatoprotective Diterpenoids from Andrographis paniculata", 《PHYTOCHEM. ANAL.》 * |
| 刘晔等: "RP-HPLC法测定穿心莲中穿心莲内酯的含量", 《解放军药学学报》 * |
| 巢志茂: "穿心莲中新的穿心莲内酯醚及抗HIV活性评价", 《国外医学中医中药分册》 * |
| 李景华等: "穿心莲二萜内酯有效部位的化学成分研究", 《河南大学学报（医学版）》 * |
| 王国才等: "穿心莲的化学成分", 《中国药科大学学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106034622A (en) * | 2016-05-31 | 2016-10-26 | 山东胜伟园林科技有限公司 | Method of drip irrigation under plastic film through employing vitamin nutrient solution, and application of method in ryegrass planting in saline and alkaline lands |
| US11191798B2 (en) | 2016-11-02 | 2021-12-07 | Nutrition Science Partners Limited | Extracts of Andrographis paniculata, methods for preparation and use thereof |
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Application publication date: 20160203 |