CN102382083A - Preparation method of andrographolide - Google Patents

Preparation method of andrographolide Download PDF

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Publication number
CN102382083A
CN102382083A CN2010102686760A CN201010268676A CN102382083A CN 102382083 A CN102382083 A CN 102382083A CN 2010102686760 A CN2010102686760 A CN 2010102686760A CN 201010268676 A CN201010268676 A CN 201010268676A CN 102382083 A CN102382083 A CN 102382083A
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preparation
alcohol
precipitate
ethanol
concentrated
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CN2010102686760A
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CN102382083B (en
Inventor
刘岩
戚可人
徐波
李伟
范开
马继忠
万晟
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TIANJIN TASLY MODERN CHINESE MEDICINE RESOURCE CO Ltd
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TIANJIN TASLY MODERN CHINESE MEDICINE RESOURCE CO Ltd
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Abstract

The invention provides a preparation method of andrographolide. The preparation method includes steps of extracting ethanol of common andrographis herb crude medicine, filtering, decolorizing by the aid of activated carbon, filtering again, concentrating cooling of a concentrated liquor, removing supernatant fluid, collecting deposit, washing the deposit by ethanol to obtain macro-crystal, dissolving the macro-crystal by ethanol, decolorizing the macro-crystal by the aid of activated carbon, filtering the macro-crystal, concentrating filtrate, recrystallizing and drying so that andrographolide is obtained. The transfer rate of andrographolide of the method is high, remained organic solvent is less, and a product is safer and effective.

Description

A kind of preparation method of rographolide
Technical field
The present invention relates to medical technical field, be specifically related to a kind of preparation method of rographolide.
Background technology
Rographolide is to extract the diterpene ginkgolide that obtains in the acanthaceous plant Herba Andrographis, is one of main effective constituent of Chinese medicine Herba Andrographis, has functions such as clearing heat and detoxicating, cool blood detumescence.
Rographolide has special efficacy to bacillary with viral upper respiratory tract infection and dysentery, is described as the natural antibiotics medicine.At present, the andrographolide preparation of State Food and Drug Administration's approval production and sales mainly contains tablet, capsule, pill etc.
The preparation of rographolide and effect bibliographical information be a lot, like Chinese patent 200710142800.7, described after a kind of alcohol extracting the method with resin isolation.Medicine Leader the 25th the 1st phase of volume of January in 2006, the progress of rographolide has been described the effect of rographolide.2002 the 19th the 3rd phases of volume of tcm-information, the rographolide process modification is inquired into the purification process of having described a kind of rographolide.2002 the 18th the 1st phases of volume of IX and absorption, macroporous adsorbent resin extracts the research of total andrographolide, has described the preparation method who crosses the rographolide of macroporous resin column behind a kind of pure drawings petroleum ether extraction.
Use during the Amberlyst process wash-out different alcoholic degree ethanol elution things all in various degree contain rographolide, 80% ethanol elution thing content is higher, but yield is lower.
Summary of the invention
The object of the present invention is to provide a kind of method of rographolide, use this method preparation to have following outstanding advantage: the rate of transform is higher, and cost is low; Do not use macroporous resin in the preparation process; Do not use organic solvents such as chloroform, acetone, sherwood oil; Reaction conditions is gentle, save energy; Product is safer and more effective, is convenient to " three wastes " and handles, and is beneficial to environment protection; The product purity that makes is high, and rographolide content can reach more than 97%; Simple operation of process is fit to industrialization production.
The invention provides a kind of preparation method of rographolide, may further comprise the steps:
(1) Herba Andrographis medicinal material extraction using alcohol;
(2) filter;
(3) use activated carbon decolorizing;
(4) filter;
(5) concentrate, concentrated liquid cooling is put, and abandoning supernatant is collected precipitate;
(6) precipitate gets coarse-grain with washing with alcohol;
(7) coarse-grain is with dissolve with ethanol, activated carbon decolorizing, filtration;
(8) concentrated, the recrystallization of filtrating, drying promptly gets.
Rographolide mainly adopts water extraction, potass extraction method, alcohol extracting method, supercritical CO in the extraction stage 2Extraction process is wherein the highest with the alcohol extracting method yield.Alcohol extracting method can be divided into impregnation technology, diacolation technology, warm soaking technology, refluxing extraction technology again, the present invention finds, putting in order of rographolide rate of transform size is impregnation technology>diacolation technology>warm soaking technology>refluxing extraction technology.Impregnation technology can be single jar of extraction of intermittent type, also can be multistage continuous extraction, and the technical application that multiple stage continuous adverse current extracts is extracted to Herba Andrographis, can obtain higher extraction efficiency, saves solvent to a greater extent, has made things convenient for subsequent operations simultaneously.
Extracting solvent can be ethanolic soln, methanol solution, acetone soln, butanone solution, and subsequent operations for ease reduces solvent contamination, most preferred ethanol solution, the preferred 50-100% of the concentration of ethanolic soln, more preferably 90-100%.
The preparation method of rographolide of the present invention comprises also between step (1) and step (2) that wherein it is 50%~60% step that water is diluted to alcohol concn with extracting solution.
The preparation method of rographolide of the present invention, wherein the concentrated of step (5) is to be evaporated to muddiness.
The preparation method of rographolide of the present invention, wherein step (6) precipitate is to use ethanolic soln, the heating or do not heat agitator treating 1-5 time.
The preparation method of rographolide of the present invention, wherein step (6) precipitate use concentration is 70%~100% ethanolic soln washing, consumption is the ethanolic soln of 0.2 times~2 times volumes of precipitate weight (L/kg).
The preparation method of rographolide of the present invention, wherein the coarse-grain of step (7) is that heated and stirred makes dissolving with the ethanolic soln more than 90% of 30 times~60 times of volumes of its weight.
The preparation method of rographolide of the present invention, wherein the concentrated of step (8) is to be evaporated to muddiness.
The preparation method of rographolide of the present invention can also comprise midbody Quality Control step between step (6) and step (7), rographolide content should be greater than 75% in the control coarse-grain.
The most preferred preparation method of the present invention may further comprise the steps:
Get the Herba Andrographis medicinal material, with the multistage continuous extraction of 90% ethanol (extract more than 3 jars, every jar of extraction at least 2 times keeps being no less than 4 times of amount extraction solvent, extracts 12 hours) at every turn at every turn, collect vat liquor, adds an amount of water, being adjusted to alcohol concn is 50%, filtration; Filtrating is heated to 60 ℃, adds proper amount of active carbon, stirs 30min, filters; Filtrate decompression is concentrated into muddiness, and concentrated liquid cooling is put, and abandoning supernatant is collected precipitate; Precipitate adds 95% ethanol of 1 times of volume of its weight (L/kg), and 60 ℃ are fully stirred down, leave standstill, and solid-liquid separation is collected solid; 95% ethanol that adds 0.5 times of volume of its weight again stirs, and leaves standstill, and solid-liquid separation gets coarse-grain; Coarse-grain adds 90% ethanolic soln of 40 times of volumes of its weight (L/kg), and 60 ℃ add proper amount of active carbon down, stir 30min, filter; Filtrate decompression is concentrated into muddiness, recrystallization, and drying promptly gets.
Advantage of the present invention:
According to the own characteristic of Herba Andrographis medicinal material, we extract the technical application that multiple stage continuous adverse current extracts to Herba Andrographis, obtain higher extraction efficiency, save solvent to a greater extent, have made things convenient for subsequent operations simultaneously.
The present invention compared with prior art, rographolide has the higher rate of transform, and has reduced organic solvent residual, product is safer and more effective.
The present invention takes the extracting mode of normal temperature lixiviate, and the effective proposition that has guaranteed rographolide is with stable.
Embodiment
Below in conjunction with embodiment the present invention is further set forth, embodiment does not just constitute any restriction to the present invention in order to make the present invention easier to understand.
Embodiment 1
Get the Herba Andrographis medicinal material, with the multistage continuous extraction of 90% ethanol (extracting 3 jars), every jar is extracted 2 times, keeps 4 times of amount extraction solvent, extracts 8 hours at every turn; Collect vat liquor, add an amount of water, being adjusted to alcohol concn is 50%, filters; Filtrating is heated to 70 ℃, adds proper amount of active carbon, stirs 30min, filters; Filtrate 70 ℃ and be concentrated into muddiness, concentrated liquid cooling is put, and abandoning supernatant is collected precipitate; Precipitate adds 0.3 times of ethanol, and 70 ℃ of stirrings are left standstill, and solid-liquid separation is collected solid; Add 0.3 times of ethanol again, stir, leave standstill, solid-liquid separation gets coarse-grain; Coarse-grain adds 30 times 90% ethanolic soln, and 70 ℃ add proper amount of active carbon, stir 30min, filter; Filtrate 70 ℃ and be evaporated to muddiness, recrystallization, drying promptly gets.
Embodiment 2
Get the Herba Andrographis medicinal material, with the multistage continuous extraction of 95% ethanol (extracting 4 jars), every jar is extracted 2 times, keeps 5 times of amount extraction solvent, extracts 12 hours at every turn; Collect vat liquor, add an amount of water, being adjusted to alcohol concn is 60%, filters; Filtrating is heated to 60 ℃, adds proper amount of active carbon, stirs 30min, filters; Filtrate 60 ℃ and be concentrated into muddiness, concentrated liquid cooling is put, and abandoning supernatant is collected precipitate; Precipitate adds 1 times of ethanol, and 55 ℃ of stirrings are left standstill, and solid-liquid separation is collected solid; Add 0.3 times of ethanol again, stir, leave standstill, solid-liquid separation gets coarse-grain; Coarse-grain adds 50 times 95% ethanolic soln, and 60 ℃ add proper amount of active carbon, stir 30min, filter; Filtrate 60 ℃ and be evaporated to muddiness, recrystallization, drying promptly gets.
Embodiment 3
Get the Herba Andrographis medicinal material, extract 2 times, extracted 12 hours at every turn with 75% alcohol dipping of 4 times of amounts; Collect vat liquor, add an amount of water, being adjusted to alcohol concn is 40%, filters; Filtrating is heated to 60 ℃, adds 0.2% gac, stirs 30min, filters; Filtrate 60 ℃ and be concentrated into muddiness, concentrated liquid cooling is put, and abandoning supernatant is collected precipitate; Precipitate adds 1 times of ethanol, stirs, and leaves standstill, and solid-liquid separation is collected solid; Add 0.5 times of ethanol again, stir, leave standstill, solid-liquid separation gets coarse-grain; Coarse-grain adds 50 times 90% ethanolic soln, and 60 ℃ add 0.2% gac, stir 30min, filter; Filtrate 60 ℃ and be evaporated to muddiness, recrystallization, drying promptly gets.
Embodiment 4
Get the Herba Andrographis medicinal material, with the multistage continuous extraction of 90% ethanol (extract more than 3 jars, every jar of extraction at least 2 times keeps being no less than 4 times of amount extraction solvent, extracts 12 hours) at every turn at every turn, collect vat liquor, adds an amount of water, being adjusted to alcohol concn is 50%, filtration; Filtrating is heated to 60 ℃, adds proper amount of active carbon, stirs 30min, filters; Filtrate decompression is concentrated into muddiness, and concentrated liquid cooling is put, and abandoning supernatant is collected precipitate; Precipitate adds 95% ethanol of 1 times of volume of its weight (L/kg), stirs, and leaves standstill, and solid-liquid separation is collected solid; 95% ethanol that adds 0.5 times of volume of its weight again, 60 ℃ are fully stirred down, leave standstill, and solid-liquid separation gets coarse-grain; Coarse-grain adds 90% ethanolic soln of 40 times of volumes of its weight (L/kg), and 60 ℃ add proper amount of active carbon down, stir 30min, filter; Filtrate decompression is concentrated into muddiness, recrystallization, and drying promptly gets.
Embodiment 5
Get the Herba Andrographis medicinal material,, collect vat liquor, filter with the multistage continuous extraction of 50% ethanol (extract more than 3 jars, every jar of extraction at least 2 times keeps being no less than 4 times of amount extraction solvent, extracts 12 hours) at every turn at every turn; Filtrating is heated to 60 ℃, adds proper amount of active carbon, stirs 30min, filters; Filtrate decompression is concentrated into muddiness, and concentrated liquid cooling is put, and abandoning supernatant is collected precipitate; Precipitate adds 95% ethanol of 0.2 times of volume of its weight (L/kg), and 60 ℃ are fully stirred down, leave standstill, and solid-liquid separation is collected solid; 95% ethanol that adds 2 times of volumes of its weight again, 60 ℃ are fully stirred down, leave standstill, and solid-liquid separation gets coarse-grain; Coarse-grain adds 95% ethanolic soln of 60 times of volumes of its weight (L/kg), and 60 ℃ add proper amount of active carbon down, stir 30min, filter; Filtrate decompression is concentrated into muddiness, recrystallization, and drying promptly gets.

Claims (10)

1. the preparation method of a rographolide may further comprise the steps:
(1) Herba Andrographis medicinal material extraction using alcohol;
(2) filter;
(3) use activated carbon decolorizing;
(4) filter;
(5) concentrate, concentrated liquid cooling is put, and abandoning supernatant is collected precipitate;
(6) precipitate gets coarse-grain with washing with alcohol;
(7) coarse-grain is with dissolve with ethanol, activated carbon decolorizing, filtration;
(8) concentrated, the recrystallization of filtrating, drying promptly gets.
2. preparation method as claimed in claim 1, wherein step (1) Herba Andrographis medicinal material extraction using alcohol adopts the alcohol dipping of 50-100% to extract.
3. preparation method as claimed in claim 2, wherein step (1) Herba Andrographis medicinal material extraction using alcohol adopts the alcohol dipping of 90-100% to extract.
4. preparation method as claimed in claim 3, wherein step (1) Herba Andrographis medicinal material extraction using alcohol adopts multiple stage continuous adverse current to extract.
5. preparation method as claimed in claim 4 comprises also between step (1) and step (2) that wherein it is 40%~70% step that water is diluted to alcohol concn with extracting solution.
6. preparation method as claimed in claim 5, wherein the concentrated of step (5) is to be evaporated to muddiness.
7. preparation method as claimed in claim 6, wherein step (6) precipitate is to use ethanolic soln, the heating or do not heat agitator treating 1-5 time.
8. preparation method as claimed in claim 7, wherein step (6) precipitate use concentration is 70%~100% ethanolic soln washing, consumption is 0.2 times~2 times volume of ethanol solution of precipitate weight.
9. preparation method as claimed in claim 7, wherein the coarse-grain of step (7) is that heated and stirred makes dissolving with the ethanolic soln more than 90% of 30 times~60 times of volumes of its weight.
10. preparation method as claimed in claim 8, wherein the concentrated of step (8) is to be evaporated to muddiness.
CN201010268676.0A 2010-09-01 2010-09-01 Preparation method of andrographolide Active CN102382083B (en)

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Cited By (13)

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Publication number Priority date Publication date Assignee Title
CN103145660A (en) * 2013-03-25 2013-06-12 成都天台山制药有限公司 Andrographolide and preparation method thereof
CN103145661A (en) * 2013-03-25 2013-06-12 成都天台山制药有限公司 New crystal form of andrographolide
CN103265509A (en) * 2013-05-28 2013-08-28 江西中医学院 Method for extracting active ingredients of andrographis paniculata in vacuum degree regulation and control auxiliary mode
CN103275042A (en) * 2013-04-23 2013-09-04 四川省裕通生物技术有限公司 Extraction and purification method for andrographolide
CN103585208A (en) * 2013-11-18 2014-02-19 华东理工大学 Preparation method of high-quality andrographolide component
CN103896890A (en) * 2014-03-04 2014-07-02 成都通德药业有限公司 Process for extracting andrographolide
CN104031011A (en) * 2014-06-30 2014-09-10 施佩蓓 Method for producing andrographolide
CN104382968A (en) * 2014-10-27 2015-03-04 南京慷睿特医药科技有限公司 Method for extracting common andrographis paniculata total lactone, pharmaceutical composition of andrographis paniculata total lactone and use of pharmaceutical composition
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
CN105153082A (en) * 2015-09-30 2015-12-16 成都中医药大学 Large-scale production technology of andrographalide
WO2018082568A1 (en) * 2016-11-02 2018-05-11 Nutrition Science Partners Limited Extracts of andrographis paniculata, methods for preparation and use thereof
CN108084122A (en) * 2018-01-30 2018-05-29 北海开元生物科技有限公司 A kind of extracting method of high-purity andrographolide
CN108236619A (en) * 2016-12-23 2018-07-03 四川文龙药业有限公司 Creat extract and its extracting method

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Cited By (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103145660B (en) * 2013-03-25 2014-09-17 成都天台山制药有限公司 Andrographolide and preparation method thereof
CN103145661A (en) * 2013-03-25 2013-06-12 成都天台山制药有限公司 New crystal form of andrographolide
CN103145661B (en) * 2013-03-25 2014-06-18 成都天台山制药有限公司 New crystal form of andrographolide
CN103145660A (en) * 2013-03-25 2013-06-12 成都天台山制药有限公司 Andrographolide and preparation method thereof
CN103275042A (en) * 2013-04-23 2013-09-04 四川省裕通生物技术有限公司 Extraction and purification method for andrographolide
CN103265509A (en) * 2013-05-28 2013-08-28 江西中医学院 Method for extracting active ingredients of andrographis paniculata in vacuum degree regulation and control auxiliary mode
CN103265509B (en) * 2013-05-28 2016-01-20 江西中医学院 A kind of method of vacuum tightness regulation and control assisted extraction Herba Andrographis activeconstituents
CN103585208A (en) * 2013-11-18 2014-02-19 华东理工大学 Preparation method of high-quality andrographolide component
CN103896890A (en) * 2014-03-04 2014-07-02 成都通德药业有限公司 Process for extracting andrographolide
CN103896890B (en) * 2014-03-04 2016-01-20 成都通德药业有限公司 A kind of extraction process of rographolide
CN104031011A (en) * 2014-06-30 2014-09-10 施佩蓓 Method for producing andrographolide
CN104382968A (en) * 2014-10-27 2015-03-04 南京慷睿特医药科技有限公司 Method for extracting common andrographis paniculata total lactone, pharmaceutical composition of andrographis paniculata total lactone and use of pharmaceutical composition
CN104382968B (en) * 2014-10-27 2021-03-30 江苏康缘药业股份有限公司 Extraction method of andrographolide, andrographolide pharmaceutical composition and application
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
CN105153082A (en) * 2015-09-30 2015-12-16 成都中医药大学 Large-scale production technology of andrographalide
WO2018082568A1 (en) * 2016-11-02 2018-05-11 Nutrition Science Partners Limited Extracts of andrographis paniculata, methods for preparation and use thereof
CN110049762A (en) * 2016-11-02 2019-07-23 营养科学合作伙伴有限公司 Andrographis Paniculata and its preparation method and application
EP3534895A4 (en) * 2016-11-02 2020-07-29 Nutrition Science Partners Limited Extracts ofandrographis paniculata
US11191798B2 (en) 2016-11-02 2021-12-07 Nutrition Science Partners Limited Extracts of Andrographis paniculata, methods for preparation and use thereof
CN108236619A (en) * 2016-12-23 2018-07-03 四川文龙药业有限公司 Creat extract and its extracting method
CN108084122A (en) * 2018-01-30 2018-05-29 北海开元生物科技有限公司 A kind of extracting method of high-purity andrographolide
CN108084122B (en) * 2018-01-30 2021-05-07 北海开元生物科技有限公司 Method for extracting high-purity andrographolide

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