CN1965896A - Prunella plant extract, preparation method, medical use and application thereof - Google Patents
Prunella plant extract, preparation method, medical use and application thereof Download PDFInfo
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- 239000000284 extract Substances 0.000 claims description 54
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- INLFWQCRAJUDCR-IQVMEADQSA-N (1R,2S,4S,5'S,6R,7S,8R,9S,12S,13S)-5',7,9,13-tetramethylspiro[5-oxapentacyclo[10.8.0.02,9.04,8.013,18]icosane-6,2'-oxane] Chemical compound O([C@@H]1[C@@H]([C@]2(CC[C@@H]3[C@@]4(C)CCCCC4CC[C@H]3[C@@H]2C1)C)[C@@H]1C)[C@]11CC[C@H](C)CO1 INLFWQCRAJUDCR-IQVMEADQSA-N 0.000 description 1
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- Medicinal Preparation (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a prunella spike extractive and relative production, wherein it uses the above-ground part of prunella spike stem and leaf as material; it uses solvent extraction method or/and acid/alkali separation method, solvent extraction method, adsorption resin method, post chromatography, concentration drying method, depressurize drying method or freeze drying method. The inventive extractive contains tuberin component as prunella spike saponin composite, while it can be made into tablet, capsule, particles, etc.
Description
[technical field]
The invention belongs to medical technical field, relate to a kind of medicinal plant extract, particularly a kind of Spica Prunellae belongs to (Prunella) plant extract, the invention still further relates to this preparation method of extract and medical usage and application.
[background technology]
The Labiatae Spica Prunellae belongs to (Prunella) plant, includes 3 mutation of 4 kinds, and Spica Prunellae wherein (P. vulgris L.) is as a kind of Chinese medicine, medically commonly used.Modern study is found, Prunella plant contains the number of chemical composition, comprise multiple compositions such as multiple triterpenoid compound, steroidal class, flavonoid, coumarin, saccharide, volatile oil and organic acid, also be used for the treatment of thyromegaly clinically mostly, lymphoid tuberculosis, cyclomastopathy, hypertension, pulmonary tuberculosis, diseases such as acute icteric infectious hepatitis.
The pharmacological research of modern medicine bound pair Prunella plant focuses mostly in its blood pressure lowering, blood sugar lowering, antiviral, effect such as antibiotic, and very limited for the research degree of depth of Prunella plant anti-mycobacterium tuberculosis, report also seldom.Only have some scattered clinical reports once to point out Spica Prunellae decocting liquid for infiltrative type, chronic fibrotic cavitys type, miliary tuberculosis of lung have certain curative effect.
Characteristics such as Spica Prunellae is because its aboundresources, and toxic and side effects is little obtain extensive use in medicine and health food.Compare with other medicines for treatment lungy, have the effect of the sharp kidney of hepatoprotective again, therefore, the research and development Spica Prunellae extract will have important pharmaceutical value and commercial value as medicine for treatment lungy.
[summary of the invention]
One of purpose of the present invention is (as the human body Liver and kidney is had toxic and side effects at the limitation that has medicine for treatment lungy now, cost an arm and a leg), and provide a kind of aboundresources, can be used for treating tuberculosis, simultaneously to human body have again the sharp kidney effect of hepatoprotective Prunella plant extract and preparation method thereof.
The object of the present invention is achieved like this:
A kind of Prunella plant extract contains prunellin (unit) compounds of anti-tubercle bacillus action activity composition.
A kind of preparation method of Prunella plant extract, it is characterized in that, be with the Labiatae Prunella plant fruit ear, stem, leaf etc. entirely in the top at least a portion be raw material, adopt solvent extraction method or with combinations such as soda acid partition method, solvent extraction, adsorption resin method, column chromatography, and be prepared from conjunction with conventional drying method such as concentrate drying, drying under reduced pressure or lyophilizations.
One of preparation method solvent extraction method.Raw material powder is broken into coarse powder, select water, alcohols (containing 1～5 carbon atom), acetone, organic ester (containing 3～6 carbon atoms), chlorinated solvents (containing 1～2 carbon atom), organic ethers (containing 3～6 carbon atoms), alkanes (containing 5～6 carbon atoms) equal solvent or two or more mixed solvents for use, dipping extracts under heating and refluxing extraction or supersound extraction or room temperature, the extraction time one or many, filter, merging filtrate, decompression and solvent recovery, dry and make extract.
Two solvent extraction methodes of preparation method+soda acid partition method.To add dilute alkaline soln according to the resulting extract of aforementioned solvents extraction method, dissolving, leach precipitation, precipitation discards, alkaline water liquid adds an amount of acid again with solution furnishing acidity, use The suitable solvent, directly extract as alcohols (containing 4～5 carbon atoms), organic ester (containing 3～6 carbon atoms), organic ethers (containing 3～6 carbon atoms), alkanes (containing 5～6 carbon atoms), extraction times can be for once, also can be repeatedly, combining extraction liquid, decompression and solvent recovery obtains Prunella plant extract.
Three solvent extraction methodes of preparation method+solvent extraction.Above-mentioned preparation method one resulting extract is suspended or be dissolved in water or the sour water, directly extract with The suitable solvent such as alcohols (containing 4～5 carbon atoms), organic ester (containing 3～6 carbon atoms), organic ethers (containing 3～6 carbon atoms), alkanes (containing 5～6 carbon atoms), extraction times can be for once, also can be repeatedly, combining extraction liquid, decompression and solvent recovery obtains Prunella plant extract.
Four solvent extraction methodes of preparation method+resin method.With moisture in the above-mentioned preparation method one or contain the extract of alcohol (containing 1～5 carbon atom) or aqueous alcohol, last macroporous adsorbent resin is handled, and discards the initial water eluent, collects pure eluting part and promptly gets extract.
Five column chromatographies of preparation method.Be silica gel column chromatography, extract with arbitrary method for preparing gained, last silicagel column, at first remove impurity such as chlorophyll with eluting such as low polar solvent such as petroleum ether, continue with two or more mixed solvent gradient elutions in suitable solvent alcohols (containing 1～5 carbon atom), organic ester (containing 3～6 carbon atoms), organic ethers (containing 3～6 carbon atoms), the alkanes (containing 5～6 carbon atoms), collection contains the eluent of active component, concentrates promptly to get extract.
Adopt said method can make Prunella plant extract, adopt the extract of the combination acquisition of diverse ways or distinct methods, some difference of concentration of component.
Described Prunella plant extract can be used as the preparation raw material of tuberculosis disease medicines such as treatment pulmonary tuberculosis, bone tuberculosis, lymphoid tuberculosis; Active component prunellin (unit) compounds in the extract or any prunellin (unit) composition also can be used as the preparation raw material of tuberculosis disease medicines such as treatment pulmonary tuberculosis, bone tuberculosis, lymphoid tuberculosis.
Described Prunella plant extract or its active component prunellin (unit) compounds or any prunellin (unit) composition, can be separately or in conjunction with or combine with suitable doctor, pharmaceutic adjuvant etc., make non-peroral dosage forms such as peroral dosage form such as tablet, capsule, granule, oral liquid or injection according to conventional method.
The present invention has following advantage:
1, the Prunella plant extract that makes in several ways of the present invention has stronger anti-tubercle bacillus activity, can further utilize the method for modern Chinese medicine, and exploitation is made for the sick class pharmaceutical preparation of a kind of natural tuberculosis.2, belong to the effect that (Prunella) plant also has the sharp kidney of hepatoprotective because of Spica Prunellae, unite use with modern tuberculosis chemicals, not only can improve the anti-tubercle bacillus curative effect, and can alleviate or eliminate because the toxic and side effects such as hepatic and renal function injure that the prolonged application chemotherapeutics is produced.3, Spica Prunellae genus (Prunella) plant resources of the present invention is abundant, low cost product; The preparation technology of extract and preparation thereof is simple, is fit to industrialization production.
[specific embodiment]
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1,2,3,4 is the preparation of Prunella plant extract, judges by the extract that makes being carried out the identification experiment, all contains prunellin (unit) compounds in all prepared products.Wherein, test 1 is acetic anhydride-strong sulfuric acid response (Liebermann-Burchard reaction), if if contain steroidal saponin in the extract, then can present dirty green, if contain triterpene saponin, then can present red, reddish violet; Test 2 if contain careless saponin (unit) compounds in the extract, then can present red or reddish violet for the strong sulfuric acid response experiment.
Among the embodiment 3, further to separating in the extract that makes, making four kinds of components (saponin (unit) class component), is respectively the 44-48 component, 50-51 component, 72-74 component, 52-62 component.
Embodiment 5 is an antibacterial experiment, take the extract that embodiment 1,2,3,4 makes, be mixed with different concentration, carry out antibacterial tests, confirm the extract that embodiment 1,2,3,4 makes, have antibacterial effect, further confirm, isolating four kinds of components among the embodiment 3 (saponin (unit) class component) show tangible tuberculosis effect, illustrate that it is the antiphthisic active component of extract.
Embodiment 6,7,8 is the medical application of Prunella plant extract.
Specific embodiment is as follows:
Embodiment 1 (solvent extraction method)
Get Spica Prunellae 400g, after spending the night with 4000mL 60% soak with ethanol, reflux, extract, 2 hours is filtered; Medicinal residues reuse 3200mL 75% ethanol is reflux, extract, 2 hours once more.Merge extracted twice liquid, add 50mL ethanol after being evaporated to about 300mL, cool, cold preservation spends the night afterwards with 4000rpm centrifugalize 20min.Get supernatant, be concentrated into 250mL, leave standstill, precipitate, get supernatant and put into refrigerator cold-storage and spend the night.Gained solution discards precipitation, getting supernatant, to be evaporated to density be 1.15, lyophilization (LGJ-10, operating pressure＜20Pa, 45 ℃), get dry thing 8.1g, yield is 2.03%, be designated as P1, judge, contain prunellin (unit) compounds in the extract by identification experiment (test 1 and test 2).Adopting ultraviolet spectrophotometry to record total saponin content is 21%.
Embodiment 2 (resin isolation method)
Get Spica Prunellae 400g, with 4000ml 90% soak with ethanol 2h, reflux, extract, 2h, filter, add 3200mL 90% ethanol in the filtering residue again, reflux, extract, 2h, filter, merge filtrate twice, being evaporated to does not have the about 420mL of alcohol flavor, gets 200mL, last macroporous adsorptive resins, wash pillar with suitable quantity of water, 40% ethanol of reuse 1340mL (2 times of column volumes) begins eluting, collects this part eluent 1120mL, reclaim solvent postlyophilization (LGJ-10, operating pressure＜20Pa, 45 ℃), get dry thing 1.48865g.Yield is 1.8%, is designated as P2, judges by identification experiment (test 1 and test 2), contains prunellin (unit) compounds in the extract.Adopting ultraviolet spectrophotometry to record total saponin content is 40%.
Embodiment 3 (adopting column chromatography) to the active component isolation identification in the Prunella plant extract
Get Spica Prunellae 2kg, with 24L ethanol lixiviate three times, each two days, filter, merge filtrate twice, being evaporated to does not have the alcohol flavor, uses petroleum ether extraction, obtains petroleum ether extract.
Petroleum ether extract is mixed sample with petroleum ether dissolution, and 100-200 order silicagel column carries out chromatography on the wet method.Earlier remove impurity such as chlorophyll, continue to adopt petroleum ether and ethyl acetate mixed solvent gradient (petroleum ether: ethyl acetate 10: the 1-ethyl acetate) eluting, Fractional Collections eluent with the petroleum ether eluting.
Get each section eluent sample, by the Tuberculosis in vitro nuclear test, and thin layer chromatography, determine that the active component position is a petroleum ether: the sample that ethyl acetate elutes at 1: 1.With petroleum ether: the sample concentration drying that ethyl acetate elutes at 1: 1 is designated as P3.Judge by identification experiment (test 1 and test 2), contain prunellin (unit) compounds in the extract.Adopt ultraviolet spectrophotometry, recording total sapogenins content is 32%.
Get an amount of P3 sample, mix sample with petroleum ether dissolution, a new 200-300 purpose silica gel pillar is proceeded chromatography on the wet method, adopt petroleum ether-ethyl acetate (4: 1-1: 2) carry out gradient elution, Fractional Collections eluent, every part of 100mL, obtain four groups of components: the 44-48 component, the 50-51 component, 72-74 component, 52-62 component.Wherein, 44-48 component, 50-51 component, 72-74 component are white powder art, and the 52-62 component is yellow sticky solid.
Differentiate and colour developing identification test by thin layer chromatography, confirm the 44-48 component, the 50-51 component, 72-74 component, 52-62 component are the sapogenin compounds.Determine that by nuclear magnetic resonance data these four kinds of components belong to oleanane type class or ursane type triterpenoid compound.
Embodiment 4 (soda acid partition method-solvent extraction)
Get Spica Prunellae 2kg, use the 24L soak with ethanol, reflux, extract, 2h, filter, add 20L ethanol, reflux, extract, 1h in the filtering residue again, filter, merge filtrate twice, be evaporated to extractum, add dilute alkaline soln, dissolving extractum, insoluble component is abandoned in filter, and it is 3 that solution is transferred pH value with concentrated hydrochloric acid, add ethyl acetate extraction 2 twice, combining extraction liquid, acetic acid ethyl acetate extract adds anhydrous sodium sulfate dehydration, and ethyl acetate is evaporated to dried, pass through thin layer chromatography, with colour developing identification test 1 and 2, be defined as prunellin (unit) class component, be designated as P5, adopt ultraviolet spectrophotometry, recording total saponins (unit) content is 38%.
The experiment of embodiment 5 Spica Prunellae extract anti-mycobacterium tuberculosis
Strain: human-like mycobacterium tuberculosis bacterial strain H37RV (deriving from Guangzhou chest hospital)
Medicine: the sample that is provided by embodiment 1-2; Rifampicin (Guangdong Huanan Pharmaceutical Factory, lot number 040502)
The preparation of pastille culture medium: is dissolution with solvents with above-mentioned medicine with water, makes the solution that concentration is 10mg/mL.With reference to the preparation method (Medical Microbiology and immunological experiment instruct) of modified Russell medium, make the pastille culture medium of concentration as shown in table 1.
Preparation of bacterium liquid and inoculation method:
Get on an amount of no medicine modified Russell medium well-grown H37RV tubercule bacillus bacterial strain after 20-30 days.It is an amount of to get above-mentioned strain, puts in the agate mortar of containing 0.5% (v/v) Tween-80 normal saline, grinds to form suspension, with turbidimetry concentration is adjusted to 1mg/mL, the dilution of reuse normal saline, and making it concentration is 0.5 * 10
-1Mg/mL uses for inoculation.Get this bacterium liquid 0.1mL, under aseptic condition, be inoculated in respectively in each culture medium of variable concentrations, make inoculation bacterium amount be about 0.5 * 10
-3Mg/mL.Put into 37 ℃ of calorstats and cultivate, begin to observe media surface colony growth situation after the week.The results are shown in following table 1:
The result of the test of table 1 Spica Prunellae grass genus plants extract Tuberculosis in vitro nuclear bacillus
| Group | Dosage (mg/ml) | After one week | After two weeks | After three weeks | All around | After eight weeks |
| P1 | 10 | - | - | - | - | - |
| 5 | - | - | - | - | - | |
| 2 | - | - | - | ++ | ++++ | |
| P2 | 10 | - | - | - | - | - |
| 5 | - | - | - | - | - | |
| 2 | - | - | + | ++ | ++++ | |
| P3 | 1 | - | - | - | - | - |
| 0.5 | - | - | - | - | - | |
| 44-48 | 0.5 | - | - | - | - | - |
| 0.1 | - | - | - | + | ++ | |
| 50-51 | 0.5 | - | - | - | - | - |
| 0.25 | - | - | - | ++ | +++ | |
| 52-62 | 0.5 | - | - | - | - | - |
| 0.25 | - | - | - | - | - | |
| 72-74 | 0.5 | - | - | - | - | - |
| 0.27 | - | - | + | ++ | +++ | |
| P5 | 1 | - | - | - | - | - |
| 0.5 | - | - | - | ++ | ++++ | |
| Blank | - | - | ++++ | ++++ | ++++ | ++++ |
| Rifampicin | 5 | - | - | - | - | - |
Annotate: the no growth of bacillus tubercle of "-" expression; "+" expression naked eyes visible colony growth, wherein+number how much reflect what of bacterium colony relative growth
Observe continuously and found that in eight weeks, blank group culture medium in two weeks shows and promptly covers with tubercule bacillus, pastille culture medium high dose group media surface in the culture experiment in eight weeks that Spica Prunellae extract P1-5 makes does not all have growth of bacillus tubercle, illustrate that Spica Prunellae extract has significant tubercle bacillus resistant activity, the saponin of column chromatography (unit) class component shows tangible tuberculosis effect, illustrates that it is the antiphthisic active component of Prunella plant extract.
Embodiment 6 Spica Prunellae powder capsules
Material: Spica Prunellae extract 300g, micropowder silica gel 6g.
Preparation: with Spica Prunellae extract, add micropowder silica gel, mixing, encapsulated, get 1000 Spica Prunellae powder capsules.
Embodiment 7 Spica Prunellae granule capsules
Material: Spica Prunellae extract 300g, Icing Sugar 40g, carboxymethyl starch sodium 8g, PVP 30g, ethanol 200ml, magnesium stearate 4g.
With Spica Prunellae extract, add Icing Sugar and carboxymethyl starch sodium, be binding agent with the ethanol liquid of PVP, encapsulated behind the system granule, 40 ℃ of dry backs and magnesium stearate mixing, 1000 of Spica Prunellae granule capsules.
Embodiment 8 Spica Prunellae Lysionotins
Material: Spica Prunellae extract 250g, Icing Sugar 100g, carboxymethyl starch sodium 8g, HMPC 6g, ethanol 200ml, magnesium stearate 2g, Pulvis Talci 2g.
With the Spica Prunellae extract fine powder, adding Icing Sugar and carboxymethyl starch sodium are binding agent with HPMC, the system granule, and dry back mixes evenly tabletting with magnesium stearate, Pulvis Talci.Promptly get 1000 of Spica Prunellae sheets.
More than be preferred forms of the present invention, according to content disclosed by the invention, some identical, replacement schemes that those of ordinary skill in the art can expect apparently all should fall into protection scope of the present invention.
Claims (9)
1, a kind of Prunella plant extract is characterized in that, contains anti-tubercle bacillus action activity composition prunellin (unit) compounds in the described extract.
2. the preparation method of a Prunella plant extract, it is characterized in that, be with Prunella plant fruit ear, stem, leaf etc. entirely in the top part be raw material, adopt solvent extraction method or with combinations such as soda acid partition method, solvent extraction, adsorption resin method, column chromatography, and be usually used in drying method in conjunction with concentrate drying, drying under reduced pressure or lyophilization etc. and be prepared from.
3, the preparation method of Prunella plant extract according to claim 2, it is characterized in that, adopt solvent extraction method: raw material powder is broken into coarse powder, select water for use, alcohols (containing 1～5 carbon atom), acetone, organic ester (containing 3～6 carbon atoms), chlorinated solvents (containing 1～2 carbon atom), organic ethers (containing 3～6 carbon atoms), alkanes (containing 5～6 carbon atoms) equal solvent or two or more mixed solvents, dipping extracts under heating and refluxing extraction or supersound extraction or room temperature, the extraction time one or many, filter, merging filtrate, decompression and solvent recovery, dry and make extract.
4, the preparation method of Prunella plant extract according to claim 2, it is characterized in that, described extract is added dilute alkaline soln, dissolving, leach precipitation, precipitation discards, alkaline water liquid adds an amount of acid again with solution furnishing acidity, use The suitable solvent, as alcohols (containing 4～5 carbon atoms), organic ester (containing 3～6 carbon atoms), organic ethers (containing 3～6 carbon atoms), alkanes (containing 5～6 carbon atoms) directly extracts, and extraction times can be for once, also can be repeatedly, combining extraction liquid, decompression and solvent recovery obtains Prunella plant extract.
5, the preparation method of Prunella plant extract according to claim 2, it is characterized in that, described extract is suspended or be dissolved in water or the sour water, use The suitable solvent, directly extract as alcohols (containing 4～5 carbon atoms), organic ester (containing 3～6 carbon atoms), organic ethers (containing 3～6 carbon atoms), alkanes (containing 5～6 carbon atoms), extraction times can be for once, also can be repeatedly, combining extraction liquid, decompression and solvent recovery obtains Prunella plant extract.
6, the preparation method of Prunella plant extract according to claim 2, it is characterized in that with described moisture or contain alcohol (containing 1～5 carbon atom) or hydrous alcohol extraction thing, last macroporous adsorbent resin is handled, discard the initial water eluent, collect pure eluting part and promptly get extract.
7, according to the preparation method of the Prunella plant extract described in the claim 2-6, it is characterized in that, with described extract, last silicagel column, at first remove impurity such as chlorophyll with eluting such as low polar solvent such as petroleum ether, continue with suitable solvent, as two or more mixed solvent gradient elutions in alcohols (containing 1～5 carbon atom), organic ester (containing 3～6 carbon atoms), organic ethers (containing 3～6 carbon atoms), the alkanes (containing 5～6 carbon atoms), collection contains the eluent of active component, concentrates promptly to get extract.
8, Prunella plant extract according to claim 1 is characterized in that, described extract can be used as the preparation raw material of tuberculosis disease medicines such as treatment pulmonary tuberculosis, bone tuberculosis, lymphoid tuberculosis; Active component prunellin (unit) compounds in the described extract or any prunellin (unit) composition also can be used as the preparation raw material of tuberculosis disease medicines such as treatment pulmonary tuberculosis, bone tuberculosis, lymphoid tuberculosis.
9, Prunella plant extract according to claim 1, it is characterized in that, described extract or its active component prunellin (unit) compounds or any prunellin (unit) composition, can be separately or in conjunction with or combine with suitable doctor, pharmaceutic adjuvant etc., make non-peroral dosage forms such as peroral dosage form such as tablet, capsule, granule, oral liquid or injection according to conventional method.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102068446A (en) * | 2011-01-10 | 2011-05-25 | 武汉道一堂医药研究院 | Application of triterpenoid saponin compound to preparation of anti-pathogeny microorganism medicament |
| CN101317883B (en) * | 2007-06-06 | 2012-01-04 | 上海中医药大学附属曙光医院 | Prunella spike active site and application of the same in preparing medicament composition |
| CN101816702B (en) * | 2009-10-13 | 2012-09-26 | 贾晓斌 | Lung cancer preventing and treating composition extracted from selfheal and/or garden orache and application thereof in preparation of lung cancer preventing and treating medicine |
| CN104815175A (en) * | 2015-04-24 | 2015-08-05 | 淄博齐鼎立专利信息咨询有限公司 | Application of traditional Chinese medicine composition in preparation of anti-tuberculin medicine |
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2006
- 2006-11-03 CN CN 200610123423 patent/CN1965896A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101317883B (en) * | 2007-06-06 | 2012-01-04 | 上海中医药大学附属曙光医院 | Prunella spike active site and application of the same in preparing medicament composition |
| CN101816702B (en) * | 2009-10-13 | 2012-09-26 | 贾晓斌 | Lung cancer preventing and treating composition extracted from selfheal and/or garden orache and application thereof in preparation of lung cancer preventing and treating medicine |
| CN102068446A (en) * | 2011-01-10 | 2011-05-25 | 武汉道一堂医药研究院 | Application of triterpenoid saponin compound to preparation of anti-pathogeny microorganism medicament |
| CN102068446B (en) * | 2011-01-10 | 2013-08-21 | 武汉道一堂医药研究院 | Application of triterpenoid saponin compound in preparation of anti-pathogeny microorganism medicament |
| CN104815175A (en) * | 2015-04-24 | 2015-08-05 | 淄博齐鼎立专利信息咨询有限公司 | Application of traditional Chinese medicine composition in preparation of anti-tuberculin medicine |
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