CN103006724A - Andrographis paniculata extract and method for preparing same - Google Patents
Andrographis paniculata extract and method for preparing same Download PDFInfo
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Abstract
The invention discloses an andrographis paniculata extract and a method for preparing the same. The andrographis paniculata extract comprises 32.3- 40.5% by mass of andrographolide and 2.23-5.52% by mass of dehydroandrographolide. The method comprises the following steps: grinding the andrographis paniculata by adopting the ball milling technology, extracting by ethanol, filtrating the obtained extract by a micro-filtration memebrane, purifying by activated carbon fiber, concentrating by a nanofiltration membrane, eluting by a macroporous resin, spraying and drying to obtain the andrographis paniculata extract. The active components such as the andrographolide in the andrographis paniculata which is a medicinal herb are kept to the maximum extent, the impurities such as the pigment in the andrographis paniculata are removed, and the strong anti-bacterial and anti-inflammatory activities of the andrographis paniculata are retained. The method of preparing the andrographis paniculata extract is easy to operate, omits the step of heating, consumes the least energy for preparation and is suitable for industrial mass production.
Description
Technical field
The present invention relates to derive from the preparation method of the medicine of plant material, be specifically related to a kind of Herba Andrographis extract and preparation method thereof.
Background technology
The Herba Andrographis medical material is acanthaceous plant Herba Andrographis
Andrographis paniculata(Burm.f.) herb of Nees has the effect of heat-clearing and toxic substances removing, removing heat from blood detumescence, and it is wide to distribute in Guangdong, and cultivation history is long.It is the raw medicinal material of the multiple famous-brand and high-quality Chinese patent medicines such as CHUANXINLIAN ZHUSHEYE, Chuanhuning preparation, andrographis tablet, XIAOYAN LIDAN PIAN, FUFANG CHUANXINLIAN PIAN.Its active component is the compositions such as andrographolide, outside this active component, also has lower other type chemical constituents such as pigment of many content.Andrographolide isoreactivity composition is subjected to thermally labile, is easy to decompose, and long-time heating can cause the structural deterioration of lactonic ring.In the preparation process of Herba Andrographis, andrographolide is in the technical process of Herba Andrographis extracting solution through concentrated and drying, and the loss rate of andrographolide and dehydrorographolide is large.In addition, other one-tenth in Herba Andrographis toxic and side effects [Academy of Military Medicine, PLA that impurity usually causes Herba Andrographis that grades, 2010, the doctorate paper, " the LIANBIZHI ZHUSHEYE safety revalues research "], Optimization Technology, the impurity component of removing tool invalid components or toxic side effect, the heat loss that reduce to extract andrographolide constituents in the concentration process are that the important topic that solves is badly in need of in the famous-brand and high-quality Chinese patent medicine manufacturer take Herba Andrographis as raw material always." creat formulation such as andrographis tablet, the XIAOYAN LIDAN PIAN etc. of Chinese pharmacopoeia (version in 2010) record, the extraction process of its Herba Andrographis raw medicinal material all is to get the alcohol extract of Herba Andrographis, adds other supplementary materials after concentrated, the drying and makes.In the production technology of its extract, the loss of andrographolide is larger, simultaneously, the active component andrographolide is not carried out purification, and the content of other compositions such as Herba Andrographis pigment is higher.
Bibliographical information is arranged to the research of the extraction process of Herba Andrographis.Such as " extraction process of creat extract ", Chinese herbal medicine 2002,6 (3): 7-9.Disclose and Herba Andrographis is put forward acid precipitation technique with alkali extracted, cost is low, the extraction efficiency of andrographolide is high, but its extraction process is complicated, easily hydrolysis in the concentration process, restive in the production, be not suitable for industrialized mass production, moreover how paper does not mention the purification andrographolide, remove the impurity components such as Herba Andrographis pigment, do not mention the concentrated, dry of extracting solution and the technology and the method that prepare its dry extract.
In addition, document " andrographolide extraction process amelioration " Chinese medicine information 2002,19(3): 50-52, mentioned the Herba Andrographis extracting solution with remove impurity with active carbon, the chloroform dissolving, the technique of acetone recrystallization is extracted the andrographolide composition, the purpose of this technique is to extract this monomer component of andrographolide, use a large amount of organic solvents in its technical process, to production safety require highly, be not suitable for equally industrialized large production.
In the Study on extraction of Herba Andrographis, the described technique of Chinese Pharmacopoeia is simple, behind 85% ethanol extraction, and extracting solution Recycled ethanol, dry getting final product.But in the present suitability for industrialized production, the concentrated drying process that all adopts single-action or the two hot concentration technologies of effect and oven dry, thereby, by its effective ingredient in the andrographis tablet of pharmacopeia explained hereafter--the total andrographolides composition has lost totally (" changes of contents of dehydrorographolide in the andrographis tablet production process " in process of production, CHINA JOURNAL OF CHINESE MATERIA MEDICA, 2002,12,36-38), this shows, this simple production Technology is not only removed impurity component, also be difficult to keep the effective ingredient in the Herba Andrographis, seriously influence the quality of creat formulation, for this reason, how further to have studied the yield of Effective Raise andrographolide isoreactivity composition, the large process for producing technology of removing to greatest extent the impurity components such as pigment has very important meaning for the quality and the curative effect that guarantee creat formulation.
Summary of the invention
The object of the present invention is to provide a kind of Herba Andrographis extract and preparation method thereof.
For solving above-mentioned deficiency, the technical scheme that the present invention takes is:
A kind of Herba Andrographis extract contains the andrographolide of mass percent 32.3～40.5% and the dehydrorographolide of mass percent 2.23～5.52%.
Preferably, described Herba Andrographis extract is chocolate brown powder.
The preparation method of above-mentioned a kind of Herba Andrographis extract, may further comprise the steps: Herba Andrographis is ground into the superfine powder granule, extract or the percolation extraction through the ethanol merceration, the Herba Andrographis extracting solution that obtains is, macroporous resin eluting purification concentrated through micro-filtrate membrane filtration, NACF column purification, NF membrane, spray drying successively, namely gets Herba Andrographis extract.
Preferably, adding volume fraction in the superfine powder granule is that 85% ethanol merceration extracts or percolation extracts, and gets the Herba Andrographis extracting solution.
Preferably, adding 10 times of bulking value marks in the superfine powder granule is that 85% ethanol merceration extracts or percolation extracts 2 times, extracts 24h at every turn, gets the Herba Andrographis extracting solution.
Preferably, adopt D101 macroporous resin eluting purification.
Preferably, by ball grinding technique Herba Andrographis is ground into the superfine powder granule.
Preferably, this preparation method, may further comprise the steps: the Herba Andrographis ball milling powder is broken into the superfine powder granule, adding 10 times of bulking value marks is that 85% ethanol merceration extracts or percolation extracts 2 times, each 24h that extracts, obtain the Herba Andrographis extracting solution through micro-filtrate membrane filtration, remove the impurity such as molecule of suspension, filtrate is passed through the NACF column purification again, remove the impurity components such as pigment, the solution after the remove impurity is through NF membrane circulation pressurization concentration and recovery ethanol, and concentrated solution is through D101 macroporous resin eluting purification, the eluent spray drying gets Herba Andrographis extract.
Described Herba Andrographis is acanthaceous plant Herba Andrographis
Andrographis paniculata(Burm.f.) herb of Nees.
This Herba Andrographis extract is take compositions such as andrographolide as its chief component, and dry product is chocolate brown powder, and flavor is extremely bitter; Its ultraviolet spectra has absorption maximum between 220～260nm; HPLC analyzes (with acetonitrile-water (18:82, v:v) gradient elution, from 0min to 60min, the concentration of acetonitrile increases to 40% from 18% linearity, flow velocity 1.0ml/min, eluent detects under the wavelength of 226nm) result shows that this active site has 7 obvious chromatographic peaks at least, wherein, andrographolide is main chromatographic peak.
The complete active component that keeps the Herba Andrographis medical material of the resulting Herba Andrographis extract of preparation method provided by the present invention, the activity that has kept the anti-inflammation of Herba Andrographis medical material, the impurity components such as pigment have effectively been removed, can add various pharmaceutic adjuvants, pharmaceutical technology routinely is prepared into various dosage forms such as granule, tablet, capsule etc.
The present invention develops Herba Andrographis extract, and the impurity contents such as andrographolide isoreactivity composition yield height wherein, pigment are low, and the integrated fabricating technology of suitability for industrialized production.Integrated fabricating technology of the present invention begins each step to the last whole technical processs such as dry run from the pulverizing of Herba Andrographis medical material, has all considered and how has effectively extracted its active component of purification.
The invention has the beneficial effects as follows:
Preparation method of the present invention is integrated preparation technology, this integrated preparation technology has kept the compositions such as active component andrographolide in the Herba Andrographis medical material to the utmost, the yield of its Antibacterial Constituents andrographolide of Effective Raise in preparation technology keeps its strong anti-inflammation active; Simultaneously, remove the impurity components such as pigment in the Herba Andrographis, avoided the generation of creat formulation toxic and side effects.
Preparation method of the present invention is comprehensive and fully take into account the effective ingredient that extracts in the purification Herba Andrographis and the purpose of removing impurity, and technique forms through Combinatorial Optimization.Adopt ball grinding technique that Herba Andrographis is ground into ultramicro powder, greatly improved the dissolution rate of andrographolide; Use percolation or merceration extractive technique, NACF column purification technology, the purification by macroporous resin technology reduces to greatest extent or removed the impurity components such as pigment in the Herba Andrographis extract.
Preparation method of the present invention need not heat can finish extraction, purification and preparation, has avoided the decomposition loss of andrographolide active component in heating process, and operation is simple and feasible, and energy consumption is low, is suitable for industrialized mass production.
The present invention is extract obtained to be characteristics according to the Herba Andrographis active component, adopted modern high technology, get through optimizing, significantly reduced the content of the impurity such as pigment in its extract, effectively kept the composition such as active component andrographolide in the Herba Andrographis medical material, can be used for preparing antibacterial-anti-inflammatory drug, such as granule, tablet, capsule etc.
Description of drawings
Fig. 1 is the HPLC chromatogram of Herba Andrographis extract AP1;
Fig. 2 is the HPLC chromatogram of Herba Andrographis extract AP2;
Fig. 3 is the HPLC chromatogram of Herba Andrographis extract AP3;
Fig. 4 is the HPLC chromatogram of Herba Andrographis extract APs.
The specific embodiment
The present invention is further illustrated below in conjunction with specific embodiment, but do not limit to so.
Following examples are mass percent if no special instructions.
The following HPLC analytical method that adopts, step is as follows: with acetonitrile-water (volume ratio 18:82) gradient elution, from 0min to 60min, the concentration of acetonitrile (volumetric concentration degree) increases to 40% from 18% linearity, flow velocity 1.0ml/min, eluent detects under the wavelength of 226nm.
Get the Herba Andrographis of 10kg, be ground into first coarse grain, then ball milling powder is broken into the superfine powder granule, extracts 2 times with 10 times of weight 85% ethanol (v/v) percolation, and each extraction time is 24h; After extracting end, filter, merge filtrate twice, obtain the Herba Andrographis extracting solution, through micro-filtration membrane (employing PP is cotton) filtration, remove the impurity such as microgranule of suspension, simultaneously, can see the PP cotton and adsorb a large amount of compositions such as pigment; Filtrate is by the NACF column purification, further remove the impurity such as pigment, solution after the purification (keeps the operating pressure of high-pressure pump between 0.6～0.9MPa) under the promotion of high-pressure pump, the Herba Andrographis extracting solution is concentrated through NF membrane circulation pressurization, be concentrated to original volume 1/10, the concentrated solution that obtains is through D101 macroporous resin (5kg) eluting purification, and the solution of collecting after the macroporous resin column carries out spray drying, namely gets Herba Andrographis extract dry powder 0.9kg (numbering: AP1).
Adopt the HPLC analytical method to measure the active component of Herba Andrographis extract dry powder AP1, the HPLC chromatogram of AP1 is seen Fig. 1, and recording Determination of Andrographolide is 40.5%, and Determination of Dehydroandrographoliin is 2.23%.
Get Herba Andrographis medical material 50kg, be ground into first coarse grain, then ball milling powder is broken into the superfine powder granule, extracts 2 times with 10 times of weight 85% ethanol (v/v) merceration, and each extraction time is 24h; After extracting end, filter, merge filtrate twice, obtain the Herba Andrographis extracting solution, through micro-filtration membrane (employing PP is cotton) filtration, remove the impurity such as microgranule of suspension, simultaneously, can see the PP cotton and adsorb a large amount of compositions such as pigment; Filtrate is by the NACF column purification, further remove the impurity such as pigment, solution after the purification (keeps the operating pressure of high-pressure pump between 0.6～0.9MPa) under the promotion of high-pressure pump, the Herba Andrographis extracting solution is concentrated through NF membrane circulation pressurization, be concentrated to original volume 1/10, the concentrated solution that obtains is through D101 macroporous resin (5kg) eluting purification, and the solution of collecting after the macroporous resin column carries out spray drying, namely gets Herba Andrographis extract dry powder 5.2 kg (numbering: AP2).The content of measuring its active component andrographolide with the HPLC analytical method is 32.3%, and the content of dehydrorographolide is 4.85%, and the HPLC collection of illustrative plates of its extract is seen Fig. 2.
Embodiment 3
Get Herba Andrographis medical material 5kg, be ground into first coarse grain, then ball milling powder is broken into the superfine powder granule, extracts 2 times with 10 times of weight 85% ethanol (v/v) percolation, and each extraction time is 24h; After extracting end, filter, merge filtrate twice, obtain the Herba Andrographis extracting solution, through micro-filtration membrane (employing PP is cotton) filtration, remove the impurity such as microgranule of suspension, simultaneously, can see the PP cotton and adsorb a large amount of compositions such as pigment; Filtrate is by the NACF column purification, further remove the impurity such as pigment, solution after the purification (keeps the operating pressure of high-pressure pump between 0.6～0.9MPa) under the promotion of high-pressure pump, the Herba Andrographis extracting solution is concentrated through NF membrane circulation pressurization, be concentrated to original volume 1/10, the concentrated solution that obtains is through D101 macroporous resin (5kg) eluting purification, and the solution of collecting after the macroporous resin column carries out spray drying, namely gets Herba Andrographis extract dry powder 0.48 kg (numbering: AP3).The content of measuring its active component andrographolide with the HPLC analytical method is 39.6%, and the content of dehydrorographolide is 5.52%, and the HPLC collection of illustrative plates of its extract is seen Fig. 3.
Comparative Examples
Get the Herba Andrographis medical material of 10kg, by " the extracting method of putting down in writing under 2010 editions one P964 andrographis tablet item of Chinese pharmacopoeia, use 85%(v/v) the ethanol hot dipping carries secondary, each 2 hours, merge extractive liquid,, filter, be concentrated between the density 1.1～1.2 with two effect concentrators, Recycled ethanol, dry in 80 ℃ of drying rooms, the Herba Andrographis extract dry powder that obtains (numbering APs), measure the active component of Herba Andrographis extract dry powder APs with the HPLC analytical method, the HPLC chromatogram of APs is seen Fig. 4, and recording Determination of Andrographolide is 4.35%, and Determination of Dehydroandrographoliin is 4.12%.
The embodiment of the invention and Comparative Examples contrast as can be known, and the present invention has improved the content of Herba Andrographis active component effectively.
Claims (8)
1. a Herba Andrographis extract contains the andrographolide of mass percent 32.3～40.5% and the dehydrorographolide of mass percent 2.23～5.52%.
2. a kind of Herba Andrographis extract according to claim 1, it is characterized in that: this extract is chocolate brown powder.
3. the preparation method of the described a kind of Herba Andrographis extract of claim 1, may further comprise the steps: Herba Andrographis is ground into the superfine powder granule, extract or the percolation extraction through the ethanol merceration, the Herba Andrographis extracting solution that obtains is, macroporous resin eluting purification concentrated through micro-filtrate membrane filtration, NACF column purification, NF membrane, spray drying successively, namely gets Herba Andrographis extract.
4. preparation method according to claim 3 is characterized in that: adding volume fraction in the superfine powder granule is that 85% ethanol merceration extracts or percolation extracts, and gets the Herba Andrographis extracting solution.
5. preparation method according to claim 4 is characterized in that: adding 10 times of bulking value marks in the superfine powder granule is that 85% ethanol merceration extracts or percolation extracts 2 times, extracts 24h at every turn, gets the Herba Andrographis extracting solution.
6. preparation method according to claim 3 is characterized in that: adopt D101 macroporous resin eluting purification.
7. preparation method according to claim 3 is characterized in that: by ball grinding technique Herba Andrographis is ground into the superfine powder granule.
8. each described preparation method according to claim 3～7, it is characterized in that: this preparation method, may further comprise the steps: the Herba Andrographis ball milling powder is broken into the superfine powder granule, adding 10 times of bulking value marks is that 85% ethanol merceration extracts or percolation extracts 2 times, each 24h that extracts, obtain the Herba Andrographis extracting solution through micro-filtrate membrane filtration, filtrate is passed through the NACF column purification again, solution after the remove impurity is through NF membrane circulation pressurization concentration and recovery ethanol, concentrated solution is through D101 macroporous resin eluting purification, the eluent spray drying gets Herba Andrographis extract.
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Cited By (10)
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| 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 |
| CN103385898A (en) * | 2013-07-24 | 2013-11-13 | 中山大学 | Method for preparing MRSA (methicillin-resistant Staphylococcus aureus)-resistant andrographis extract |
| CN104140403A (en) * | 2014-07-02 | 2014-11-12 | 成都通德药业有限公司 | Andrographolide separation and purification process |
| CN104557819A (en) * | 2014-12-19 | 2015-04-29 | 浙江大学 | Method for preparing andrographolide and application of andrographolide |
| CN105062686A (en) * | 2015-07-17 | 2015-11-18 | 王再青 | Method for extracting lavender essential oil |
| CN106616028A (en) * | 2016-12-08 | 2017-05-10 | 西南大学 | Viral disease preventing and curing feed additive for cyprinus carpio and preparation method thereof |
| CN108815213A (en) * | 2018-08-27 | 2018-11-16 | 维康腾达生物科技有限公司 | A kind of preparation method of Andrographis Paniculata |
| CN113045520A (en) * | 2021-03-25 | 2021-06-29 | 江西新世纪民星动物保健品有限公司 | Extraction process of andrographolide |
| US11191798B2 (en) | 2016-11-02 | 2021-12-07 | Nutrition Science Partners Limited | Extracts of Andrographis paniculata, methods for preparation and use thereof |
| CN113970605A (en) * | 2021-10-13 | 2022-01-25 | 江苏协合转化医学研究院有限公司 | Method for screening active substances in abelmoschus manihot |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN103385898A (en) * | 2013-07-24 | 2013-11-13 | 中山大学 | Method for preparing MRSA (methicillin-resistant Staphylococcus aureus)-resistant andrographis extract |
| CN104140403A (en) * | 2014-07-02 | 2014-11-12 | 成都通德药业有限公司 | Andrographolide separation and purification process |
| CN104140403B (en) * | 2014-07-02 | 2015-12-09 | 成都通德药业有限公司 | A kind of separation purifying technique of rographolide |
| CN104557819A (en) * | 2014-12-19 | 2015-04-29 | 浙江大学 | Method for preparing andrographolide and application of andrographolide |
| CN105062686A (en) * | 2015-07-17 | 2015-11-18 | 王再青 | Method for extracting lavender essential oil |
| US11191798B2 (en) | 2016-11-02 | 2021-12-07 | Nutrition Science Partners Limited | Extracts of Andrographis paniculata, methods for preparation and use thereof |
| CN106616028A (en) * | 2016-12-08 | 2017-05-10 | 西南大学 | Viral disease preventing and curing feed additive for cyprinus carpio and preparation method thereof |
| CN108815213A (en) * | 2018-08-27 | 2018-11-16 | 维康腾达生物科技有限公司 | A kind of preparation method of Andrographis Paniculata |
| CN113045520A (en) * | 2021-03-25 | 2021-06-29 | 江西新世纪民星动物保健品有限公司 | Extraction process of andrographolide |
| CN113970605A (en) * | 2021-10-13 | 2022-01-25 | 江苏协合转化医学研究院有限公司 | Method for screening active substances in abelmoschus manihot |
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