CN101332229A - Prunella plant extract, preparation method and use thereof - Google Patents
Prunella plant extract, preparation method and use thereof Download PDFInfo
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- CN101332229A CN101332229A CNA2008100329719A CN200810032971A CN101332229A CN 101332229 A CN101332229 A CN 101332229A CN A2008100329719 A CNA2008100329719 A CN A2008100329719A CN 200810032971 A CN200810032971 A CN 200810032971A CN 101332229 A CN101332229 A CN 101332229A
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Abstract
The invention relates to prunella plant extract which comprises total phenolic acid extracts forming active ingredients; in the total phenolic acid extracts, the content of rosmarinic acid is 21.5-65.0wt%, and the content of total phenolic acid is 70.5-99.0wt%. The prunella plant extract also contains total triterpene extracts forming the active ingredients; in the total triterpene extracts, the content of ursolic acid is 10.0-45.0wt%, and the content of total triterpene is 50.5-98.0wt%. The invention also relates to a preparation method of the composition and the application in the medicine.
Description
Technical field
The present invention relates to from plant, extract and contain extraction of active ingredients thing and this preparation method of extract and the new purposes of this extract in medicine.Relate in particular to from Prunella plant, to extract and contain the extraction of active ingredients thing.The invention still further relates to this preparation method of extract and their medicinal usage.
Background technology
The Labiatae Prunella plant whole world has 15 kinds, in home-made mainly containing: Spica Prunellae Prunella vulgaris L., Herba Ajugae P.vulgaris L.var.leucantha Schur sec.bailey, narrow leaf Spica Prunellae P.vulgaris L.var.leucantha (Barton) Fernald, french spinach P.asiatica Nakai., its mutation P.asiatica Nakai var.albiflora (koidz.) Nakai, bristle Spica Prunellae P.hispida Benth., Prunella grandiflora P.gramdiflora (linn.) Jacq..As Chinese medicine commonly used be drying and ripening fruit ear or the herb of Spica Prunellae Prunella vulgarls L. wherein, have relieve inflammation or internal heat, make eye bright, the effect of eliminating stagnation, detumescence, be used for that conjunctival congestion and swelling pain, order pearl carbuncle at night, headache are dizzy, pyogenic infection of the pad of a finger scrofula, carcinoma and relieving mammary gland gall, thyromegaly, diseases such as tuberculous lymphadenitis, cyclomastopathy, hypertension.The single preparation of Spica Prunellae has Spica Prunellae oral liquid, Spica Prunellae granule etc. in the market, what be Spica Prunellae slightly obtains through refining agent, extraction process is coarse, and quality controllability is not strong, does not see that up to the present the effective site of the Spica Prunellae that clearer and more definite chemical constituent is arranged is declared as new drug.
Mainly contain triterpene and compositions such as glycoside, sterol and glycoside thereof, flavonoid, coumarin, phenolic acid, volatile oil and saccharide thereof in the Prunella plant.Wherein based on the triterpenes components of ursolic acid, oleanolic acid with based on the liposoluble ingredient of rosmarinic acid, caffeic acid, content is the main effective ingredient of Spica Prunellae than horn of plenty.The bibliographical information Spica Prunellae has multiple effects such as blood pressure lowering, blood fat reducing, antiinflammatory, immunosuppressant, antibiotic, antiviral, blood sugar lowering, antitumor, effects such as that rosmarinic acid has is antibiotic, antiviral, antiinflammatory, antioxidation, immunosuppressant, antiallergic, anti-platelet aggregation, ursolic acid has multiple pharmacological activities such as antitumor, anti-liver injury, anti-inflammation and antiviral.
Spica Prunellae oral liquid mainly for treating mammary gland hypertrophy disease and hypertension, clinical experience proof determined curative effect for many years.Cyclomastopathy is relevant with hypothalamus～hypophysis～ovary～mammary gland endocrine axis disorder, be the result of multiple endocrine hormone imbalance, wherein estrogenic/progestogenic out of proportion make mammary gland under estrogenic stimulation the essence hypertrophy excessively and subinvolution be one of most important reason.Chinese medicine thinks that this disease belongs to due to stagnation of QI due to depression of the liver, phlegm and blood stasis, the disharmony of Chong and Conception Channels; Stagnation of QI due to depression of the liver, the expectorant stasis of blood are handed over and are hindered in the mark of newborn network for disease, deficiency of kidney-QI dash, appoint imbalance for sick originally.
Though the pharmacological action report to Spica Prunellae is more, the material base of its pharmacological action is which chemical position and which pharmacological action are associated not fully aware of.The present invention tries hard to from the modern thinking of Chinese medicine, understands fully the main chemical position in the Prunella plant and the relation of corresponding drug effect, makes it meet the requirement of modern drug development " safe, effective, quality controllable ".
Aspect patent documentation, Granted publication is number for CN1331488C discloses " a kind of Spica Prunellae extract and purposes ", and the content of the total phenolic acid of active component is 60～70% in the disclosed Spica Prunellae extract of this Chinese patent, and the content of rosmarinic acid is 14～21%; This patent also discloses the application of its extract in preparation rheumatoid arthritis medicine in addition.
Publication number is that CN1965896A discloses " a kind of Prunella plant extract and preparation method and medical usage and application ", in the disclosed Spica Prunellae extract of this patent application, its active component is prunellin (unit) compounds that contains the tuberculosis effect, and this patent also discloses its extract and can be used as application in the tuberculosis disease medicines such as treatment pulmonary tuberculosis, bone tuberculosis, lymphoid tuberculosis in addition.
Publication number is CN101040905A disclosed " with the hypoglycemic drug of Spica Prunellae preparation ", and this patent points out that Spica Prunellae total triterpenic acids content is more than or equal to 50% in medicine.
Summary of the invention
Technical problem first aspect to be solved by this invention provides a kind of Prunella plant extract, the specific chemical components of said extracted thing, quality controllable, be easy to carry out the deep pharmacology of system, study of pharmacy, meet the requirement of the modernization of Chinese medicine " safe, effective, quality controllable ".
Technical problem second aspect to be solved by this invention is at the deficiencies in the prior art, has proposed the preparation method of above-mentioned Prunella plant extract, has improved the content that can measure chemical constituent in the extract, makes it be more suitable for being used for medicinal usage.
The technical problem third aspect to be solved by this invention provides the medicinal usage of above-mentioned Prunella plant extract.
As the Prunella plant extract of first aspect present invention, comprise the total phenolic acid extract that constitutes active component, wherein in total phenolic acid extract, the single component rosmarinic acid contents is 21.5～65.0wt%, total phenolic content is 70.5～99.0wt%.
In the Prunella plant extract of the present invention, also comprise the total-triterpene extract that constitutes active component, wherein in total-triterpene extract, the single component content of ursolic acid is 10.0～45.0wt%, and total triterpene contents is 50.5～98wt%.
It is 100: 1～1: 100 as the weight ratio between active component total phenolic acid extract and the total-triterpene extract in the Prunella plant extract of the present invention.Wherein preferred weight ratio is 3: 1.
Preparation method as the total phenolic acid extract in the Prunella plant extract of second aspect present invention comprises following steps:
(1) gets the fruit ear or the herb of Prunella plant, use ethanol extraction, collect each alcohol extract, filter the back and merge; The alcohol extract that merges reclaims ethanol, refilter filtering residue and filtrate A;
(2) after filtrate A concentrates, add acid for adjusting pH to 2～6, use ethyl acetate extraction, get ethyl acetate layer and reclaim ethyl acetate, residue is total phenolic acid extract.
In above-mentioned steps (1), when using ethanol extraction, the alcoholic acid weight percent concentration of employing is 40～100%.In preferred embodiment of the present invention, alcoholic acid weight percent concentration is 80%.
In above-mentioned steps (1), when using ethanol extraction, make a living 2～10 times of volumes of dose of each consumption.Be preferably 7 times of volumes.
In above-mentioned steps (1), when using ethanol extraction, extraction time is 1～4 time, and each extraction time is 1～3 hour.Preferred number of times is 3 times, and extraction time was followed successively by 2,1.5,1 hours.
In above-mentioned steps (1), employing reflux mode is extracted or is adopted ultrasonic power to extract.
In above-mentioned steps (1), adopt the concentrating under reduced pressure mode to reclaim ethanol, be concentrated into 1 times of volume of about crude drug amount.
In above-mentioned steps (1), before filtering, increase by is the standing over night step at room temperature.
In above-mentioned steps (2), filtrate A is concentrated into 1/10～2 times of volume of crude drug amount.Preferably be concentrated into 1/2 volume.
In above-mentioned steps (2), selected acid is a kind of in acetic acid, formic acid, the hydrochloric acid.Be preferably 0.1N hydrochloric acid.
In above-mentioned steps (2), pH value is preferably 3.
In above-mentioned steps (2), with ethyl acetate extraction three times, make a living 1/2 volume of dose of the consumption of each ethyl acetate.
In above-mentioned steps (2), before reclaiming ethyl acetate, increase a combined ethyl acetate layer, the step of washing with the saturated nacl aqueous solution of 1/5 volume of crude drug amount.
In above-mentioned steps (2), in the described total phenolic acid extract, the content of rosmarinic acid is 21.5～65.0wt%, and total phenolic content is 70.5～99.0wt%.
Preparation method as the total-triterpene extract in the Prunella plant extract of second aspect present invention comprises following steps:
(a) get the fruit ear or the herb of Prunella plant, use ethanol extraction, collect each alcohol extract, filter the back and merge; The alcohol extract that merges reclaims ethanol, refilter filtering residue A and filtrate;
(b) filtering residue A with organic solvent dissolution after, add kieselguhr and mix sample absorption, carry out column chromatography after the drying, earlier with low polar organic solvent washing defat, reuse Semi-polarity or the strong total triterpene of polar organic solvent eluting;
(c) total triterpene eluent decompression and solvent recovery, the residue dissolve with ethanol adds acid for adjusting pH to 3～6.5, adds the active carbon reflux again or stirs decolouring, filter, filtrate recycling ethanol, residue is total-triterpene extract.
In above-mentioned steps (a), when using ethanol extraction, the alcoholic acid weight percent concentration of employing is 40～100%.In preferred embodiment of the present invention, alcoholic acid weight percent concentration is 80%.
In above-mentioned steps (a), when using ethanol extraction, make a living 2～10 times of volumes of dose of each consumption.Be preferably 7 times of volumes.
In above-mentioned steps (a), when using ethanol extraction, extraction time is 1～4 time, and each extraction time is 1～3 hour.Preferred number of times is 3 times, and extraction time is 2,1.5,1 hours successively.
In above-mentioned steps (a), employing reflux mode is extracted or is adopted ultrasonic power to extract.
In above-mentioned steps (a), adopt the concentrating under reduced pressure mode to reclaim ethanol, be concentrated into 1 times of volume of about crude drug amount.
In above-mentioned steps (a), before filtering, increase by is the standing over night step at room temperature.
In above-mentioned steps (b), the organic solvent of dissolving filtering residue A is selected a kind of or its mixing in ethanol, acetone, the ethyl acetate for use.Be preferably ethanol.When being preferably ethanol, make a living 1/50～1/2 volume of dose of consumption.Be preferably 1/5 volume.Alcoholic acid weight percent concentration is 80～100%.Preferred weight percent concentration is 80%.
In above-mentioned steps (b), the kieselguhr specification is selected a kind of or its mixing in 50 orders～500 orders for use.Preferred 100 order kieselguhr.Make a living 1/50～1/2 weight of dose of described kieselguhr consumption is preferably 1/10 weight.
In above-mentioned steps (b), the low polar organic solvent of selecting for use is a kind of or its mixing in petroleum ether, ether, the hexane.Be preferably petroleum ether.When being preferably petroleum ether, the consumption of petroleum ether be used crude drug amount 1/4～4 times of volume.Be preferably 1 times of volume.
In above-mentioned steps (b), Semi-polarity of selecting for use or strong polar organic solvent are a kind of or its mixing in acetone, ethyl acetate, ethanol, the methanol.Be preferably ethanol.When being preferably ethanol, its consumption is 1/4～4 times of volume of used crude drug amount.Preferred 1 times of volume.
In above-mentioned steps (c), described residue weight percent concentration is 80～95% dissolve with ethanols, make a living 1/10～2 times of volume of dose of consumption of ethanol.Be preferably 1/2 volume.
In above-mentioned steps (c), selected acid is a kind of in acetic acid, formic acid, the hydrochloric acid.Be preferably acetic acid.
In above-mentioned steps (c), pH value is preferably 5.
In above-mentioned steps (c), make a living 1/500～1/10 weight of dose of the addition of active carbon.Be preferably 1/100 weight.
In above-mentioned steps (c), the time of active carbon reflux or stirring decolouring is 0.5～2 hour.Be preferably 1 hour.
In above-mentioned steps (c), increase a total-triterpene extract and wash exsiccant then step with water 1～3 time, make a living 1/100～1 times of volume of dose of each water consumption.Be preferably with the water washing of crude drug amount 1/10 volume 2 times.
In above-mentioned steps (c), in the resulting total-triterpene extract, content of ursolic acid is 10.0～45.0wt%, and total triterpene contents is 50.5～98.0wt%.
As the medicinal usage of the above-mentioned Prunella plant extract of third aspect present invention be with the total phenolic acid extract in the described Prunella plant extract or/and total-triterpene extract as active component, add acceptable accessories, the medicine of any dosage form of making.Preferred dosage form is the tablet or the capsule of oral administration.
Above-mentioned Prunella plant extract is as follows as the concrete medicinal usage of active component, but is not limited to following medicinal usage:
1, can be in the application in preparation prevention and the treatment cyclomastopathy medicine with Prunella plant extract as active component.
2, can be in the application in preparation prevention and the treatment thyroid medicine with Prunella plant extract as active component.
3, can be in the application in preparation prevention and the treatment pulmonary tuberculosis medicine with Prunella plant extract as active component.
4, can be in the application in preparation prevention and the treatment medicaments for coronary disease with Prunella plant extract as active component.
5, can be in the application in preparation prevention and the treatment angina drug with Prunella plant extract as active component.
6, can be in the application in preparation prevention and the treatment hypertension disease medicament with Prunella plant extract as active component.
7, can be in the application in preparation prevention and the treatment hyperglycemia medicine with Prunella plant extract as active component.
8, can be in the application in preparation prevention and the treatment cervical erosion medicine with Prunella plant extract as active component.
9, can be in the application in the preparation extensive pedigree antibiotic with Prunella plant extract as active component.
The content height of total phenolic acid in the Prunella plant extract of the present invention, it is having better curative effect aspect treatment cyclomastopathy, thyroid, pulmonary tuberculosis, coronary heart disease, angina pectoris, hypertension, hyperglycemia, cervical erosion, the disease such as antibiotic.The extraction of Prunella plant extract of the present invention, it is simple to have a processing step, yield height, eco-friendly advantage.
The specific embodiment
Prunella plant extract of the present invention contains the total phenolic acid of active component or/and total-triterpene extract, and indication is extensive.This Prunella plant extract can be made tablet, capsule, pill, the agent of powder art, suppository and solution and suspending agent according to the known method of pharmaceuticals industry, wherein preferably is fit to the capsule and the tablet of gastrointestinal administration.When preparation is fit to the capsule, tablet, pill of oral administration and powder agent, can use sucrose, lactose, galactose, corn starch, gelatin, microcrystalline Cellulose, carboxymethyl cellulose etc. as carrier or excipient.
In addition, also can use in the pharmaceuticals industry known method and auxiliary element medicine of the present invention to be made solution and the suspending agent that is suitable for oral administration.In order to prepare solution and the suspending agent that is suitable for the outer administration of gastrointestinal tract, can use distilled water, water for injection, isotonic sodium chlorrde solution or glucose solution, perhaps (for example 1～100mM) phosphate buffer (PBS) is as carrier or diluent for low concentration.Can add one or more other auxiliary elements or additives in the preparation of these gastrointestinal tract external administrations, for example can use ascorbic acid as antioxidant, use sodium benzoate etc. are as antiseptic.Solubilizing agent, disintegrating agent, lubricant, coloring agent, dispersant or the surfactant that in the preparation of these dosage forms, can also contain other.
The present invention is described further below in conjunction with specific embodiment, but do not limit the present invention in any way.
Embodiment 1
The preparation method of the total phenolic acid extract in the Prunella plant extract:
(1) Spica Prunellae fruit ear 500g, adding the weight percent concentration is that 80% ethanol adopts the reflux mode to extract three times, each 3500ml, the time was followed successively by 2,1.5,1 hours; Merge three times extracting solution, adopt the method for concentrating under reduced pressure to reclaim ethanol, be concentrated into about 500ml; At room temperature standing over night is filtered, and filtering residue A and filtrate A be standby filtering residue A respectively, the dry about 12g in back;
(2) filtrate A is concentrated into about 250ml, add the 0.1N dilute hydrochloric acid and transfer pH to 3, with ethyl acetate extraction 3 times, each ethyl acetate consumption is 250ml, gets ethyl acetate layer, with the washing of 100ml saturated nacl aqueous solution, reclaim ethyl acetate, get total phenolic acid extract 10.1g, wherein rosmarinic acid contents 33%, total phenolic content 84%.
Embodiment 2
The preparation method of the total phenolic acid extract in the Prunella plant extract:
(1) Spica Prunellae fruit ear 100g, adding the weight percent concentration is that 80% ethanol adopts ultransonic method to extract three times, each 700ml, the time was followed successively by 2,1.5,1 hours.Merge three times extracting solution, adopt the method for concentrating under reduced pressure to reclaim ethanol, be concentrated into about 100ml; At room temperature standing over night is filtered, and filtering residue A and filtrate A are standby respectively; About 2.5g after the filtering residue A drying.
(2) filtrate A is concentrated into about 50ml, add the 0.1N dilute hydrochloric acid and transfer PH to 3, with ethyl acetate extraction 3 times, each ethyl acetate consumption is 50ml, gets ethyl acetate layer, with the washing of 20ml saturated nacl aqueous solution, reclaim ethyl acetate, get total phenolic acid extract 2.1g, wherein rosmarinic acid contents 34%, total phenolic content 82%.
Embodiment 3
The preparation method of the total phenolic acid extract in the Prunella plant extract:
(1) Spica Prunellae fruit ear 100g, adding the weight percent concentration is that 80% ethanol adopts ultransonic method to extract three times, each 700ml, the time was followed successively by 2,1.5,1 hours; Merge three times extracting solution, adopt the method for concentrating under reduced pressure to reclaim ethanol, be concentrated into about 100ml; At room temperature standing over night is filtered, and filtering residue A and filtrate A are standby respectively, about 2.6g after the filtering residue A drying;
(2) filtrate A is concentrated into about 50ml, add the 0.1N dilute hydrochloric acid and transfer PH to 3, with ethyl acetate extraction 3 times, each ethyl acetate consumption is 50ml, gets ethyl acetate layer, with the washing of 20ml saturated nacl aqueous solution, reclaim ethyl acetate, get total phenolic acid extract 2.3g, wherein rosmarinic acid contents 31%, total phenolic content 79%.
Embodiment 4
The preparation method of the total phenolic acid extract in the Prunella plant extract:
(1) Spica Prunellae fruit ear 100g, adding the weight percent concentration is that 80% ethanol adopts the reflux mode to extract three times, each 700ml, the time was followed successively by 2,1.5,1 hours.Merge three times extracting solution, adopt the method for concentrating under reduced pressure to reclaim ethanol, be concentrated into about 100ml; At room temperature standing over night is filtered, and filtering residue A and filtrate A are standby respectively, about 2.5g after the filter residue and drying;
(2) filtrate A is concentrated into about 50ml, adds formic acid and transfers PH to 3, uses ethyl acetate extraction 3 times, and each ethyl acetate consumption is 50ml, reclaims ethyl acetate, gets total phenolic acid extract 2.5g, and wherein rosmarinic acid contents 23%, total phenolic content 72%.
Embodiment 5
The preparation method of the total phenolic acid extract in the Prunella plant extract
(1) Spica Prunellae herb 100g, adding the weight percent concentration is 50% ethanol ultrasonic extraction 2 times, each 1000ml, the time was followed successively by 2,1.5 hours.Merge extractive liquid, adopts the method for concentrating under reduced pressure to reclaim ethanol, is concentrated into about 100ml; At room temperature standing over night is filtered, and filtering residue A and filtrate A are standby respectively, about 2.4g after the filter residue and drying;
(2) filtrate A is concentrated into about 50ml, add formic acid and transfer PH to 2, with ethyl acetate extraction 3 times, each ethyl acetate consumption is 50ml, gets ethyl acetate layer, with the washing of 20ml saturated nacl aqueous solution, reclaim ethyl acetate, get total phenolic acid extract 2.3g, wherein rosmarinic acid contents 24%, total phenolic content 75%;
Embodiment 6
The preparation method of the total phenolic acid extract in the Prunella plant extract:
(1) Spica Prunellae herb 100g, adding the weight percent concentration is 95% ethanol ultrasonic extraction 4 times, each 500ml, the time was followed successively by 2.5,1.5,1,1 hours.Merge extractive liquid, adopts the method for concentrating under reduced pressure to reclaim ethanol, is concentrated into about 100ml; At room temperature standing over night is filtered, and filtering residue A and filtrate A are standby respectively, about 2.8g after the filter residue and drying;
(2) filtrate A is concentrated into about 100ml, add formic acid and transfer PH to 6, with ethyl acetate extraction 3 times, each ethyl acetate consumption is 100ml, gets ethyl acetate layer, with the washing of 20ml saturated nacl aqueous solution, reclaim ethyl acetate, get total phenolic acid extract 1.8g, wherein rosmarinic acid contents 23%, total phenolic content 73%.
Embodiment 7
The preparation method of the total-triterpene extract in the Prunella plant extract:
(1) the filtering residue A weight percent concentration of getting embodiment 1 is the about 100ml dissolving of 80% ethanol, adds 100 order kieselguhr 50g and mixes sample absorption, and evaporated under reduced pressure is carried out column chromatography, with petroleum ether 500ml eluting, reclaim petroleum ether, abandon residue, reuse ethanol 500ml eluting is collected total triterpene eluent;
(2) total triterpene eluent decompression recycling ethanol gets residue 4.6g, is 90% ethanol 250ml dissolving with weight percent concentration, adds acetic acid adjust pH to 5, adds active carbon 5g reflux decolouring 1 hour; Filter, filtrate recycling ethanol gets total-triterpene extract 2.8g, and wherein ursolic acid content 32%, total triterpene contents 68%;
Embodiment 8
The preparation method of the total-triterpene extract in the Prunella plant extract:
(1) the filtering residue A weight percent concentration of getting embodiment 2 is the about 20ml dissolving of 80% ethanol, add 100 order kieselguhr 10g and mix sample absorption, volatilize ethanol, evaporated under reduced pressure is carried out column chromatography, with petroleum ether 100ml eluting, reclaim petroleum ether, abandon residue, reuse ethanol 100ml eluting is collected total triterpene eluent;
(2) total triterpene eluent decompression recycling ethanol gets residue 0.95g, with weight percent concentration be? % ethanol 50ml dissolving adds acetic acid adjust pH to 5, adds 1g active carbon reflux decolouring 1 hour; Filter, filtrate recycling ethanol, residue wash with water 2 times, and about at every turn 10ml filters, and dry filtering residue gets total-triterpene extract 0.59g, and wherein ursolic acid content 30%, total triterpene contents 66%.
Embodiment 9
The preparation method of the total-triterpene extract in the Prunella plant extract:
(1) the filtering residue A weight percent concentration of getting embodiment 3 is the about 20ml dissolving of 80% ethanol, add 100 order kieselguhr 10g and mix sample absorption, volatilize ethanol, evaporated under reduced pressure is carried out column chromatography, with petroleum ether 100ml eluting, reclaim petroleum ether, abandon residue, reuse ethanol 100ml eluting is collected total triterpene eluent;
(2) total triterpene eluent decompression recycling ethanol gets residue 0.95g, is 90% ethanol 50ml dissolving with weight percent concentration, adds acetic acid adjust pH to 5, adds 1g active carbon reflux decolouring 1 hour; Filter, filtrate recycling ethanol, residue wash with water 2 times, and about at every turn 10ml filters, and dry filtering residue gets total-triterpene extract 0.59g, and wherein ursolic acid content 29%, total triterpene contents 63%.
Embodiment 10
The preparation method of the total-triterpene extract in the Prunella plant extract:
(1) getting embodiment 4 filtering residue A weight percent concentration is the about 20ml dissolving of 60% ethanol, adds 100 order kieselguhr 10g and mixes sample absorption, volatilizes ethanol, evaporated under reduced pressure is carried out column chromatography, with petroleum ether 100ml eluting, reclaims petroleum ether, abandon residue, reuse acetone 100ml eluting is collected total triterpene eluent;
(2) total triterpene eluent reclaim under reduced pressure acetone gets residue 0.82g, is 90% ethanol 50ml dissolving with weight percent concentration, and ice acetic acid adjust pH to 5 adds 1g active carbon reflux decolouring 1 hour; Filter, filtrate recycling ethanol, residue wash with water 2 times, and about at every turn 10ml filters, and dry filtering residue gets total-triterpene extract 0.51g, and wherein ursolic acid content 28%, total triterpene contents 67%.
Embodiment 11
The preparation method of the total-triterpene extract in the Prunella plant extract:
(1) the filtering residue A weight percent concentration of getting embodiment 5 is the about 20ml dissolving of 50% ethanol, add 100 order kieselguhr 10g and mix sample absorption, volatilize ethanol, evaporated under reduced pressure is carried out column chromatography, with ether 100ml eluting, reclaim ether, abandon residue, reuse ethyl acetate 100ml eluting is collected total triterpene eluent;
(2) total triterpene eluent reclaim under reduced pressure ethyl acetate gets residue 0.84g, is 95% ethanol 25ml dissolving with weight percent concentration, adds acetic acid adjust pH to 3, adds 1g active carbon heated and stirred decolouring 1 hour, and heating-up temperature is 50 ℃; Filter, filtrate recycling ethanol, residue wash with water 2 times, and about at every turn 10ml filters, and dry filtering residue gets total-triterpene extract 0.49g, and wherein ursolic acid content 25%, total triterpene contents 64%.
Embodiment 12
The preparation method of the total-triterpene extract in the Prunella plant extract:
(2) the filtering residue A weight percent concentration of getting embodiment 6 is the about 20ml dissolving of 95% ethanol, add 100 order kieselguhr 10g and mix sample absorption, volatilize ethanol, evaporated under reduced pressure is carried out column chromatography, with ether 100ml eluting, reclaim ether, abandon residue, reuse ethyl acetate 100ml eluting is collected total triterpene eluent;
(3) total triterpene eluent reclaim under reduced pressure ethyl acetate gets residue 0.90g, is 80% ethanol 100ml dissolving with weight percent concentration, adds acetic acid adjust pH to 6.5, adds 1g active carbon reflux decolour 2 hours; Filter, filtrate recycling ethanol, residue wash with water 2 times, and about at every turn 10ml filters, and dry filtering residue gets total-triterpene extract 0.55g, and wherein ursolic acid content 22%, total triterpene contents 60%.
Embodiment 13
A kind of Prunella plant total phenolic acid extract assay:
(1) rosmarinic acid contents is measured
Experimental apparatus: high performance liquid chromatogram instrument, Tianjin, island
HPLC condition: enlightening horse C
18Jewel post; Methanol: 0.1% acetic acid, 80: 20; Flow velocity 1ml/min; 25 ℃ of column temperatures; Detect wavelength 280nm.
The preparation of reference substance liquid:
Take by weighing rosmarinic acid reference substance (content 98%, Nat'l Pharmaceutical ﹠ Biological Products Control Institute) 9.75mg and add dissolve with methanol in the 10ml measuring bottle, methanol constant volume shakes up to scale, gets in 1ml to the 10ml measuring bottle, and methanol constant volume shakes up to scale, promptly.
The preparation of test sample liquid:
Take by weighing self-control Spica Prunellae total phenolic acids extract 26.42mg in the 25ml measuring bottle, add dissolve with methanol, methanol constant volume shakes up to scale, gets in 1ml to the 10ml measuring bottle, and methanol constant volume shakes up to scale, crosses 0.45 μ m microporous filter membrane, promptly.
Experimental technique and result:
Each 20 μ l sample introduction of reference substance liquid and test sample liquid are measured the rosmarinic acid peak area, calculate that rosmarinic acid contents is 33% in the Spica Prunellae total phenolic acids extract.
(2) total phenolic content is measured
Experimental apparatus: 756MC ultraviolet-uisible spectrophotometer, Shanghai Precision Scientific Apparatus Co., Ltd
The preparation of reference substance liquid:
Measure item reference substance liquid down with rosmarinic acid contents.
The preparation of test sample liquid:
Measure item test sample liquid down with rosmarinic acid contents.
Experimental technique and result:
Pipette methanol (blank), reference substance liquid and each 2ml of test sample liquid respectively, to conical flask, respectively add 5% sodium nitrite solution 0.5ml, place 5min, add 10% aluminum nitrate solution 0.5ml, place 5min, add 1N sodium hydroxide solution 5ml again, shake up, place 15min, measure trap at 500nm wavelength place.
Record in the Spica Prunellae total phenolic acids extract total phenolic content and count 84% with protocatechualdehyde.
Embodiment 14
A kind of Prunella plant total-triterpene extract assay:
(1) ursolic acid content is measured
Experimental apparatus: the high performance liquid chromatogram instrument, Agilent 1100
HPLC condition: enlightening horse C
18Jewel post; Methanol: 0.1% acetic acid, 90: 10; Flow velocity 1ml/min; 35 ℃ of column temperatures; Detect wavelength 210nm.
The preparation of reference substance liquid:
Take by weighing ursolic acid reference substance (content 98%, Nat'l Pharmaceutical ﹠ Biological Products Control Institute) 21.79mg and add dissolve with methanol in the 25ml measuring bottle, methanol constant volume shakes up to scale, promptly.
The preparation of test sample liquid:
Take by weighing self-control Spica Prunellae total triterpenes extract 20.63mg in the 10ml measuring bottle, add dissolve with methanol, methanol constant volume shakes up to scale, crosses 0.45 μ m microporous filter membrane, promptly.
Experimental technique and result:
Each 20 μ l sample introduction of reference substance liquid and test sample liquid are measured the ursolic acid peak area, calculate that ursolic acid content is 32% in the Spica Prunellae total triterpenes extract.
(2) total triterpene contents is measured
Experimental apparatus: 756MC ultraviolet-uisible spectrophotometer, Shanghai Precision Scientific Apparatus Co., Ltd
The preparation of reference substance liquid:
Get ursolic acid content and measure in following reference substance liquid 1ml to the 10ml measuring bottle, methanol constant volume shakes up to scale, promptly.
The preparation of test sample liquid:
Get ursolic acid content and measure in following test sample liquid 1ml to the 10ml measuring bottle, methanol constant volume is got in 1ml to the 10ml measuring bottle to scale, and methanol constant volume shakes up to scale, promptly.
Experimental technique and result:
Pipette methanol (blank), reference substance liquid and each 0.6ml of test sample liquid respectively, to tool plug test tube, volatilize solvent, respectively add 10% sulphuric acid vanillin reagent 0.4ml, perchloric acid 1ml, inaccessible 60 ℃ of water-bath 15min, ice bath 2min immediately, ice acetic acid 5ml shakes up, and measures trap at 546nm wavelength place.
Record in the Spica Prunellae total triterpenes extract total triterpene contents and count 68% with ursolic acid.
Embodiment 15
A kind of Prunella plant extract only contains the capsular preparation of total phenolic acid extract
Get the Prunella plant extract 120g that only contains total phenolic acid extract, with microcrystalline Cellulose 130g mixing, spray ethanol 40ml stirs, and makes granule, and drying incapsulates, and makes 1000, promptly.
Every capsules loading amount 250mg.Contain total phenolic acid and be not less than 84mg, rosmarinic acid is not less than 26mg.
Embodiment 16
A kind of Prunella plant extract contains total phenolic acid extract and the capsular preparation of total-triterpene extract
Get Spica Prunellae total phenolic acids extract 90g, total-triterpene extract 30g forms the extract combination of being made up of Spica Prunellae total phenolic acids and total triterpene.Again with sieve after 130g microcrystalline Cellulose mixing, spray ethanol 40ml stirs, and makes granule, drying incapsulates, and makes 1000, promptly.
Every capsules loading amount 250mg.Contain ursolic acid and be not less than 6mg, total triterpene is not less than 15mg; Containing rosmarinic acid is not less than 18mg and contains total phenolic acid and be not less than 63mg.
Embodiment 17
A kind of Prunella plant extract only contains the preparation of total phenolic acid extract tablet
Get the Prunella plant extract 120g that only contains total phenolic acid extract, with microcrystalline Cellulose 100g, starch 20g, magnesium stearate 10g mixing, spray ethanol 40ml, mixing is granulated, and is pressed into 1000, promptly.
Every heavy 250mg.Contain rosmarinic acid and be not less than 26mg, total phenolic acid is not less than 84mg.
Embodiment 18
A kind of Prunella plant extract contains the preparation of total phenolic acid extract and total-triterpene extract tablet
Get withered total careless total-triterpene extract 30g of summer, total phenolic acid extract 90g forms the extract combination of being made up of Spica Prunellae total triterpenes and Spica Prunellae total phenolic acids.With microcrystalline Cellulose 100g, starch 20g, magnesium stearate 10g mixing, spray ethanol 40ml again, mixing is granulated, and is pressed into 1000, promptly.
Every heavy 250mg.Contain ursolic acid and be not less than 3mg, total triterpene is not less than 15mg; Contain rosmarinic acid and be not less than 19mg, total phenolic acid is not less than 63mg.
Embodiment 19
The compositions of Prunella plant extract is to the pharmacological action of cyclomastopathy rat
Withered total careless total-triterpene extract of summer (being called for short A), total phenolic acid extract (being called for short B), Spica Prunellae total triterpenes and Spica Prunellae total phenolic acids are pressed different proportion and are mixed the extract combination of forming (being called for short XKC).
Get female unpregnancy SD rat, intramuscular injection estradiol benzoate 0.5mg/kg/ days continues 20 days, uses instead Progesterone 4mg/kg/ days, continuous 5 days, causes the rat mammary gland model of hyperplasia.During the modeling, irritate stomach every day and give total-triterpene extract, total phenolic acid extract and a certain proportion of Spica Prunellae extract combination (2g/kg), the model control group animal is taken 0.9% normal saline, the oral tamoxifen 0.5mg/kg/ of positive controls days.Other establishes the normal control group.Behind the successive administration 30 days, put to death animal, win the 2nd pair of complete mammary gland tissue, row HE dyeing, the om observation mammary gland tissue is learned performance.
Sign is observed: compares with the normal control group, and model control group nipple redness, mammary gland increases obviously, and the sign of each administration group then approaches normal control.The microscopy observed result is as shown in table 1.
Table 1. Spica Prunellae extract to the influence of mammary gland tissue (x ± s, n=10)
Annotate: compare with model control group,
*P＜0.05,
*P＜0.01.
Embodiment 20
The compositions of Prunella plant extract is to the pharmacological action of the big mice of Iodine excess goiter
Get the Kunming kind healthy mice of just weaning, male and female half and half freely supply to drink the negative control group drinking public water supply with the drinking water that contains KI 3000ug/ml.Simultaneously, irritate stomach every day and give total-triterpene extract, total phenolic acid extract and the combination of a certain proportion of Spica Prunellae extract (2g/kg) or normal saline.After 120 days, win thyroid and weigh, calculate the enlargement rate.The result is as shown in table 3.
Table 2. Spica Prunellae extract to the influence of thyromegaly and weight (x ± s, n=12)
Annotate: compare with model control group,
*P＜0.05,
*P＜0.01.
Embodiment 21
The application of Prunella plant extract aspect tuberculosis treatment
Adopt two times of gradient dilution methods of traditional test tube, in modified Russell medium, inoculate the human-like mycobacterium tuberculosis type strain of people's pulmonary tuberculosis pathogenic bacterium H37RV, mycobacterium bovis respectively, (bacteria concentration is 10 to Mycobacterium phlei 0.5ml
5CFU/ml), add total-triterpene extract, total phenolic acid extract and combination of a certain proportion of Spica Prunellae extract or solvent control again, and in 37 ℃ of incubators, hatch 30d, observe respectively being subjected to the minimal inhibitory concentration (MIC) of test solution antibacterial.See table 9 for details.These results show that Prunella plant extract is effective to phthisical prevention and treatment.
Table 3. Prunella plant extract is to the MIC of all kinds of tubercule bacillus
Embodiment 22
The compositions of Prunella plant extract is to the protective effect of myocardial ischemia reperfusion injury
Adopt isolated rat perfusion heart (Langendorff heart) ischemia-reperfusion injury model, with the K～HShi buffer perfused hearts that contains total-triterpene extract, total phenolic acid extract and the combination of a certain proportion of Spica Prunellae extract, detect in the cardiac muscular tissue MDA content and irritate LDH activity in the 15min perfusate again, this two indexes can reflect and the closely-related oxygen-derived free radicals level variation of myocardial damage indirectly.Chamber incidence rate of quivering of each group of record.Pour into result such as the table 5 that causes again, shown in 6,7.
Table 4. Spica Prunellae extract to isolated rat perfusion heart chamber quiver incidence rate influence (x ± s, n=12)
Annotate: compare with negative control group,
*P＜0.05,
*P＜0.01.
Table 5. Spica Prunellae extract to isolated myocardium organize MDA content influence (x ± s, n=12)
Annotate: compare with negative control group,
*P＜0.05,
*P＜0.01.
Table 6. Spica Prunellae extract to irritate again the active influence of LDH in the perfusate (x ± s, n=12)
Annotate: compare with negative control group,
*P＜0.05,
*P＜0.01.
Embodiment 23
The compositions of Prunella plant extract is to the pharmacological action of renal vascular hypertension rat
Adopt two kidneys, one folder legal system to do 70 of successful renal vascular hypertension rats, be divided into 7 groups at random, model group, Captopril group (Cap, 3mg/kg), total-triterpene extract group, total phenolic acid extract group and a certain proportion of Spica Prunellae extract combination group (2g/kg).Gastric infusion, the model group physiologic saline for substitute.Adopt RBP～I type blood pressure heart rate measuring instrument to survey arteria caudalis systolic pressure and the heart rate of rat under the waking state.Before the record administration (0min), 10min after the administration, 30min, 60min, 90min, the systolic pressure of 120min and 150min and heart rate.The result shows that heart rate does not have significant change, and systolic pressure changes as shown in table 4.
Table 7. Spica Prunellae extract to the influence of Hypertensive Rats systolic pressure (x ± s, n=10)
Annotate: compare with model control group,
*P＜0.05,
*P＜0.01.
Embodiment 24
The compositions of Prunella plant extract is to the blood sugar reducing function of diabetic mice
Get Kunming mouse, tail vein injection alloxan normal saline solution (80mg/kg), posterior orbit was got the hematometry fasting glucose in 96 hours.Blood glucose value＞20mmol/L, simultaneously with polydipsia, polyuria symptom as diabetes modeling success mice.Diabetic mice is divided into model group, metformin group, total-triterpene extract group, total phenolic acid extract group and a certain proportion of Spica Prunellae extract combination group, and other establishes the normal control group.Adopt and irritate stomach mode administration or normal saline, continuous 14 days.Before administration, the 7th day, the 14th day morning the fasting glucose measured with blood glucose meter, also exempted from method mensuration serum insulin levels on the 14th day with putting.The result is as shown in table 8.
Table 8. Spica Prunellae extract to the influence of blood glucose in diabetic mice and insulin (x ± s, n=10)
Annotate: compare with model control group,
*P＜0.05,
*P＜0.01.
Embodiment 25
Prunella plant extract is to the effect of cervical erosion rat
Get 60 of Healthy female rats, be divided into normal group, model group, total triterpene group, total phenolic acid group and Spica Prunellae extract combination group (4g/kg, 1: 3) at random.Make the cervical erosion rat with phenol rubber cement injection model group and each treated animal vagina of XKC.Irritate stomach in molding success back and give XKC or normal saline, 1 time/day, continuous 20 days.Put to death animal, get its cervical tissue through HE dyeing row histopathologic examination.Perusal is found, the cervical tissue hyperemia of model group, and edema is obvious.Microscopic examination finds that cell infiltration is serious under the model group cervix uteri mucosa, congestion of blood vessel expansion, and mucosa ulcer has appearred in minority; Spica Prunellae extract combination group (4g/kg, 1: 3) group mucosa is complete substantially, only a small amount of inflammatory cell under mucosa and the mucosa, and epithelial cell degeneration necrosis number significantly is lower than model group; Total triterpene group, total phenolic acid group can be improved inflammatory symptom, reduce the ulcer area, but effect are not as good as Spica Prunellae extract combination group (4g/kg, 1: 3).Generally speaking, Prunella plant extract treatment cervical erosion has certain curative effect.
Embodiment 26
The bacteriostatic activity test of Prunella plant extract
Total triterpene group, total phenolic acid group and Spica Prunellae extract combination group (4g/kg, 1: 3) are added Nutrient agar or husky Bao Shi agar or blood agar culture-medium, pour plate with two times of gradient dilution method dilution backs.Select for use with urologic disease, strain (staphylococcus aureus, staphylococcus epidermidis, streptococcus faecalis, gonococcus, escherichia coli, gardnerella vaginalis, proteus vulgaris, Candida albicans) that gynaecopathia is relevant and become 1 * 10
9The concentration of individual/ml is got 1 ring with inoculating loop and is coated on the pastille flat board, puts 37 ℃ of incubators and cultivates (gonococcus is put 37 ℃ of CO2 gas incubator, and white the thought put 28 ℃ of incubators).Observe 16-48 hour cultivation results (as shown in table 10).The result shows that Prunella plant extract all has broad-spectrum antibacterial action, and is effective to the main pathogenic bacterium of urinary system relevant disease, gynaecopathia.
The fungistatic effect of table 9 Prunella plant extract
Claims (66)
1. Prunella plant extract, it is characterized in that: comprise the total phenolic acid extract that constitutes active component, wherein in total phenolic acid extract, rosmarinic acid contents is 21.5～65.0wt%, total phenolic content is 70.5～99.0wt%.
2. Prunella plant extract as claimed in claim 1, it is characterized in that: also comprise the total-triterpene extract that constitutes active component, wherein in total-triterpene extract, content of ursolic acid is 10.0～45.0wt%, and total triterpene contents is 50.5～98.0wt%.
3. Prunella plant extract as claimed in claim 2 is characterized in that: as the weight ratio between active component total phenolic acid extract and the total-triterpene extract is 100: 1～1: 100.
4. Prunella plant extract as claimed in claim 2 is characterized in that: as the weight ratio between active component total phenolic acid extract and the total-triterpene extract is 3: 1.
5. Prunella plant extract as claimed in claim 1 or 2 is characterized in that being selected from a kind of in the following Prunella plant or their combination: Spica Prunellae, Herba Ajugae, narrow leaf Spica Prunellae, french spinach and mutation thereof, bristle Spica Prunellae, Prunella grandiflora.
6. method for preparing the described total phenolic acid extract of claim 1 is characterized in that: comprise following steps:
(1) gets the fruit ear or the herb of Prunella plant, use ethanol extraction, collect each alcohol extract, filter the back and merge; The alcohol extract that merges reclaims ethanol, refilter filtering residue A and filtrate A;
(2) after filtrate A concentrates, add acid for adjusting pH to 2～6, use ethyl acetate extraction, get ethyl acetate layer and reclaim ethyl acetate, residue is total phenolic acid extract.
7. method according to claim 6 is characterized in that: in described step (1), when using ethanol extraction, the alcoholic acid weight percent concentration of employing is 40～100%.
8. method according to claim 6 is characterized in that: in described step (1), when using ethanol extraction, the alcoholic acid weight percent concentration of employing is 80%.
9. method according to claim 6 is characterized in that: in described step (1), and when using ethanol extraction, make a living 2～10 times of volumes of dose of each consumption.
10. method according to claim 6 is characterized in that: in described step (1), and when using ethanol extraction, make a living 7 times of volumes of dose of each consumption.
11. method according to claim 6 is characterized in that: in described step (1), when using ethanol extraction, extraction time is 1～4 time, and each extraction time is 1～3 hour.
12. method according to claim 6 is characterized in that: in described step (1), when using ethanol extraction, extraction time is 3 times, and extraction time was followed successively by 2,1.5,1 hours.
13. method according to claim 6 is characterized in that: in described step (1), adopt the reflux mode or adopt ultrasonic power to extract.
14. method according to claim 6 is characterized in that: in described step (1), adopt the concentrating under reduced pressure mode to reclaim ethanol, be concentrated into 1 times of volume of about crude drug amount.
15. method according to claim 6 is characterized in that: in described step (1), before filtering, increase by is the standing over night step at room temperature.
16. method according to claim 6 is characterized in that: in described step (2), filtrate A is concentrated into 1/10～2 times of volume of crude drug amount.
17. method according to claim 6 is characterized in that: in described step (2), filtrate A is concentrated into 1/2 volume of crude drug amount.
18. method according to claim 6 is characterized in that: in described step (2), selected acid is a kind of in acetic acid, formic acid, the hydrochloric acid.
19. method according to claim 6 is characterized in that: in described step (2), selected acid is 0.1N hydrochloric acid.
20. method according to claim 6 is characterized in that: in described step (2), pH value is 3.
21. method according to claim 6 is characterized in that: in described step (2), with ethyl acetate extraction three times, make a living 1/2 volume of dose of the consumption of each ethyl acetate.
22. method according to claim 6 is characterized in that: in described step (2), before reclaiming ethyl acetate, increase a combined ethyl acetate layer, the step of washing with the saturated nacl aqueous solution of 1/5 volume of crude drug amount.
23. method according to claim 6 is characterized in that: in described step (2), in the described total phenolic acid extract, the content of rosmarinic acid is 21.5～65.0wt%, and total phenolic content is 70.5～99.0wt%.
24. a method for preparing the described total-triterpene extract of claim 2 is characterized in that: comprise following steps:
(1) gets the fruit ear or the herb of Prunella plant, use ethanol extraction, collect each alcohol extract, filter the back and merge; The alcohol extract that merges reclaims ethanol, refilter filtering residue A and filtrate A;
(2) filtering residue A with organic solvent dissolution after, add kieselguhr and mix sample absorption, carry out column chromatography after the drying, earlier with low polar organic solvent washing defat, reuse Semi-polarity or the strong total triterpene of polar organic solvent eluting;
(3) total triterpene eluent decompression and solvent recovery, the residue dissolve with ethanol adds acid for adjusting pH to 3～6.5, adds the active carbon reflux again or stirs decolouring, filter, filtrate recycling ethanol, residue is total-triterpene extract;
25. method according to claim 24 is characterized in that: in described step (1), when using ethanol extraction, the alcoholic acid weight percent concentration of employing is 40～100%.
26. method according to claim 24 is characterized in that: in described step (1), when using ethanol extraction, the alcoholic acid weight percent concentration of employing is 80%.
27. method according to claim 24 is characterized in that: in described step (1), when using ethanol extraction at every turn, make a living 2～10 times of volumes of dose of consumption.
28. method according to claim 24 is characterized in that: in described step (1), when using ethanol extraction at every turn, make a living 7 times of volumes of dose of consumption.
29. method according to claim 24 is characterized in that: in described step (1), when using ethanol extraction, extraction time is 1～4 time, and each extraction time is 1～3 hour.
30. method according to claim 24 is characterized in that: in described step (1), when using ethanol extraction, extraction time is 3 times, and extraction time was followed successively by 2,1.5,1 hours.
31. method according to claim 24 is characterized in that: in described step (1), employing reflux mode is extracted or is adopted ultrasonic power to extract.
32. method according to claim 24 is characterized in that: in described step (1), adopt the concentrating under reduced pressure mode to reclaim ethanol, be concentrated into 1 times of volume of about crude drug amount.
33. method according to claim 24 is characterized in that: in described step (1), before filtering, increase by is the standing over night step at room temperature.
34. method according to claim 24 is characterized in that: in described step (2), the organic solvent of dissolving filtering residue A is selected a kind of or its mixture in ethanol, acetone, the ethyl acetate for use.
35. method according to claim 34 is characterized in that: when selecting ethanol for use, make a living 1/50～1/2 volume of dose of described ethanol consumption; Described alcoholic acid weight percent concentration is 80～100%.
36. method according to claim 35 is characterized in that: make a living 1/5 volume of dose of described ethanol consumption; Described alcoholic acid weight percent concentration is 80%.
37. method according to claim 24 is characterized in that: in described step (2), the kieselguhr specification is selected a kind of or its mixing in 50 orders～500 orders for use; Make a living 1/50～1/2 weight of dose of described kieselguhr consumption.
38. method according to claim 24 is characterized in that: in described step (2), the kieselguhr specification is selected 100 orders for use; Make a living 1/10 weight of dose of described kieselguhr consumption.
39. method according to claim 24 is characterized in that: in described step (2), the low polar organic solvent of selecting for use is a kind of or its mixture in petroleum ether, ether, the hexane.
40. according to the described method of claim 39, it is characterized in that: when the low polar organic solvent of selecting for use was petroleum ether, the consumption of petroleum ether was 1/4～4 times of volume of used crude drug amount.
41. according to the described method of claim 39, it is characterized in that: when the low polar organic solvent of selecting for use was petroleum ether, the consumption of petroleum ether was 1 times of volume of used crude drug amount.
42. method according to claim 24 is characterized in that: in described step (2), Semi-polarity of selecting for use or strong polar organic solvent are a kind of or its mixture in acetone, ethyl acetate, ethanol, the methanol.
43. according to the described method of claim 42, it is characterized in that: when Semi-polarity of selecting for use or strong polar organic solvent were ethanol, its consumption was 1/4～4 times of volume of used crude drug amount.
44. according to the described method of claim 42, it is characterized in that: when Semi-polarity of selecting for use or strong polar organic solvent were ethanol, its consumption was 1 times of volume of used crude drug amount.
45. method according to claim 24 is characterized in that: in described step (3), described residue weight percent concentration is 80～95% dissolve with ethanols, make a living 1/10～2 times of volume of dose of consumption of ethanol.
46., it is characterized in that: make a living 1/2 volume of dose of described consumption of ethanol according to the described method of claim 45.
47. method according to claim 24 is characterized in that: in described step (3), selected acid is a kind of in acetic acid, formic acid, the hydrochloric acid.
48. method according to claim 24 is characterized in that: in described step (3), pH value is 5.
49. method according to claim 24 is characterized in that: in described step (3), make a living 1/500～1/10 weight of dose of the addition of active carbon.
50. method according to claim 24 is characterized in that: in described step (3), make a living 1/100 weight of dose of the addition of active carbon.
51. method according to claim 24 is characterized in that: in described step (3), the time of reflux or stirring decolouring is 0.5～2 hour.
52. method according to claim 24 is characterized in that: the time of reflux or stirring decolouring is 1 hour.
53. method according to claim 24 is characterized in that: in described step (3), increase a total-triterpene extract and wash exsiccant then step with water 1～3 time, make a living 1/100～1 times of volume of dose of each water consumption.
54. method according to claim 24 is characterized in that: in described step (3), the step of the washing total-triterpene extract of increase be wash with water 2 times dry then, make a living 1/10 volume of dose of each water consumption.
55. method according to claim 24 is characterized in that: in described step (3), in the resulting total-triterpene extract, content of ursolic acid is 10.0～45.0wt%, and total triterpene contents is 50.5～98.0wt%.
56. the medicinal usage of the described Prunella plant extract of claim 1 be with described Prunella plant extract as active component, add acceptable accessories, the medicine of any dosage form of making.
57. the medicinal usage of the described Prunella plant extract of claim 2 be with described Prunella plant extract as active component, add acceptable accessories, the medicine of any dosage form of making.
58. the purposes according to claim 56 or 57 is characterized in that: described dosage form is the tablet or the capsule of oral administration.
59. can be as active component in the application in preparation prevention and the treatment cyclomastopathy medicine as the described Prunella plant extract of claim 1～2.
60. can be as active component in the application in preparation prevention and the treatment thyroid medicine as the described Prunella plant extract of claim 1～2.
61. can be as active component in the application in preparation prevention and the treatment pulmonary tuberculosis medicine as the described Prunella plant extract of claim 1～2.
62. can be as active component in the application in preparation prevention and the treatment medicaments for coronary disease as the described Prunella plant extract of claim 1～2.
63. can be as active component in the application in preparation prevention and the treatment angina drug as the described Prunella plant extract of claim 1～2.
64. can be as active component in the application in preparation prevention and the treatment hypertension disease medicament as the described Prunella plant extract of claim 1～2.
65 can be in the application in preparation prevention and the treatment hyperglycemia medicine as active component as the described Prunella plant extract of claim 1～2.
66. can be as active component in the application in preparation prevention and the treatment cervical erosion medicine as the described Prunella plant extract of claim 1～2.
67. can be as active component in the application in the preparation extensive pedigree antibiotic as the described Prunella plant extract of claim 1～2.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101862373A (en) * | 2010-06-12 | 2010-10-20 | 广州星群（药业）股份有限公司 | Quality control method for mulberry chrysanthemum granules |
| CN102432469A (en) * | 2011-12-08 | 2012-05-02 | 刘正芳 | Method for extracting and separating rosmarinic acid and ursolic acid from rosemary |
| CN106727928A (en) * | 2017-01-18 | 2017-05-31 | 天津大学 | Prunella vulgaris extract and preparation method and application |
| FR3077732A1 (en) * | 2018-02-15 | 2019-08-16 | Robertet | PROCESS FOR OBTAINING ROSMARINIC ACID ENRICHED EXTRACT FROM FRESH VEGETABLE MATERIAL |
| CN111166789A (en) * | 2019-11-28 | 2020-05-19 | 湖南中医药大学 | Application of Prunella vulgaris flower extract in preparing medicine for treating liver injury |
| CN111358833A (en) * | 2020-04-22 | 2020-07-03 | 贵阳新天药业股份有限公司 | Prunella vulgaris extract and application thereof in preparation of medicines for treating thyroid diseases |
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| CN1331488C (en) * | 2004-02-18 | 2007-08-15 | 江苏康缘药业股份有限公司 | Prunella spike extract and its preparation method and use |
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2008
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101862373A (en) * | 2010-06-12 | 2010-10-20 | 广州星群（药业）股份有限公司 | Quality control method for mulberry chrysanthemum granules |
| CN101862373B (en) * | 2010-06-12 | 2012-01-04 | 广州星群（药业）股份有限公司 | Quality control method for mulberry chrysanthemum granules |
| CN102432469A (en) * | 2011-12-08 | 2012-05-02 | 刘正芳 | Method for extracting and separating rosmarinic acid and ursolic acid from rosemary |
| CN106727928A (en) * | 2017-01-18 | 2017-05-31 | 天津大学 | Prunella vulgaris extract and preparation method and application |
| FR3077732A1 (en) * | 2018-02-15 | 2019-08-16 | Robertet | PROCESS FOR OBTAINING ROSMARINIC ACID ENRICHED EXTRACT FROM FRESH VEGETABLE MATERIAL |
| WO2019158654A1 (en) | 2018-02-15 | 2019-08-22 | Robertet | Method for obtaining an extract enriched in rosmarinic acid from fresh plant matter |
| US11458179B2 (en) | 2018-02-15 | 2022-10-04 | Plantes Aromatiques Du Diois | Method for obtaining an extract enriched in rosmarinic acid from fresh plant material |
| CN111166789A (en) * | 2019-11-28 | 2020-05-19 | 湖南中医药大学 | Application of Prunella vulgaris flower extract in preparing medicine for treating liver injury |
| CN111358833A (en) * | 2020-04-22 | 2020-07-03 | 贵阳新天药业股份有限公司 | Prunella vulgaris extract and application thereof in preparation of medicines for treating thyroid diseases |
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