CN102205000A - Callicarpa nudiflora Hook. et Arn. extract, preparation method and application thereof - Google Patents
Callicarpa nudiflora Hook. et Arn. extract, preparation method and application thereof Download PDFInfo
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- CN102205000A CN102205000A CN2010105084749A CN201010508474A CN102205000A CN 102205000 A CN102205000 A CN 102205000A CN 2010105084749 A CN2010105084749 A CN 2010105084749A CN 201010508474 A CN201010508474 A CN 201010508474A CN 102205000 A CN102205000 A CN 102205000A
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Abstract
Relating to the field of traditional Chinese medicine preparation, the invention provides a Callicarpa nudiflora Hook. et Arn. extract, and its preparation method and application. Containing flavonoid and water-soluble ingredients, the Callicarpa nudiflora Hook. et Arn. extract is characterized by additionally containing diterpene and triterpene fat-soluble ingredients. The Callicarpa nudiflora Hook. et Arn. extract of the invention is extracted by supersonic waves for preparing bacteriostatic, antiphlogistic, hemostatic and astringent medicaments. The beneficial effect of the extract provided in the invention is that: not only containing flavonoid, tannin and other water-soluble ingredients, but also containing diterpene and triterpene fat-soluble ingredients, the extract of the invention has more complete active ingredients and a comparatively increased content, thus being beneficial to the application of various preparations. Requiring no heating, the preparation method of the invention is energy saving and of high extraction rate.
Description
Technical field
The present invention relates to field of traditional Chinese medicine pharmacy, be specifically related to the purposes of extract, this preparation method of extract and this extract of a kind of Callicarpa nudiflora plant.
Background technology
Callicarpa nudiflora is the dried leaves of Verenaceae plant Callicarpa nudiflora, be used as medicine hemostasis is arranged, antibiotic, convergence, detoxifcation, analgesia and the effect that promotes healing.The main component of Callicarpa nudiflora is water-soluble components such as flavonoid, diterpene and triterpenoid compound, condensed tannins, phenols, polysaccharide, hydroxy compounds and magnesium, calcium, iron salt, wherein, flavonoid comprises verbascoside, luteolin and luteoloside etc., general flavone content is up to about 5%, diterpene and triterpenoid compound comprise ursolic acid and oleanolic acid etc., relevant bibliographical information and experimental result show that part triterpene, flavone compound in the Callicarpa nudiflora leaf ethanol extract have significant analgesia role to mice.
Only contain flavone compound, tannin class and some other water soluble ingredient in the existing Callicarpa nudiflora extract, and extracting method adopts traditional heat reflow method usually, be about to Callicarpa nudiflora and decoct with water after-filtration, concentrated, the dry extract that gets, this method wastes time and energy, expend the energy, and most fat-soluble active ingredient can not extract.
Summary of the invention
The objective of the invention is provides a kind of Callicarpa nudiflora extract that comprises ursolic acid and verbascoside at top described defective.
Another object of the present invention provides a kind of preparation method of Callicarpa nudiflora extract and a kind of purposes of Callicarpa nudiflora extract.
Purpose of the present invention is achieved by the following technical programs.
A kind of Callicarpa nudiflora extract comprises flavone compound, water soluble ingredient, it is characterized in that: also include diterpene, triterpenes liposoluble constituent.
Described diterpene, triterpenes liposoluble constituent comprise a kind of in pier fruit acid, the ursolic acid at least; Flavone compound comprises a kind of in luteolin, luteolin glycosides, the verbascoside at least.
Index components is to indicate with ursolic acid content and verbascoside content in the extract of the present invention.Ursolic acid content is not less than 0.92%; Verbascoside content is not less than 1.37%.
A kind of preparation method of Callicarpa nudiflora extract is characterized in that: may further comprise the steps.
1) Callicarpa nudiflora is pulverized medical material doubly to measure concentration with 7-9 is 70-90% soak with ethanol 60-90min, 30-50min is extracted with the ultrasonic extraction device in the back, filter then, filtering residue adds 3-5 again, and doubly to measure concentration be 70-90% soak with ethanol 60-90min, 15-25min is extracted with the ultrasonic extraction device in the back, filtration also merges filtrate twice, and 1. the ethanol that reclaims in the filtrate get extractum.
2) filtering residue crossed of above-mentioned ethanol extraction is a solvent with 8-12 times of water gaging again, extracts 30-50min with the ultrasonic extraction device, filter afterwards, aqueous extract behind concentrating under reduced pressure extractum 2..
3) merge extractum 1. with extractum 2., be condensed into thick paste under the vacuum, with thick paste dry to moisture below 5%, Callicarpa nudiflora extract.
That extract of the present invention is used to prepare is antibacterial, antiinflammatory, hemostasis, analgesia and astringent medicine.
Extract of the present invention can be prepared into preparation with the adjuvant that pharmaceutically allows to use.
It is the single preparations of ephedrine of principal agent that the present invention can be made into the Callicarpa nudiflora extract.
The present invention can be made into the compound preparation that contains Callicarpa nudiflora extract.
The present invention can be made into solid preparation (granule, capsule, tablet, dispersible tablet, powder, pill), liquid preparation (soft capsule, mixture, oral liquid, syrup), the external preparation (suppository, ointment, ointment) that contains Callicarpa nudiflora extract.
The invention has the beneficial effects as follows: not only contain water soluble ingredients such as flavonoid, tannin class in the extract of the present invention, and contain diterpene, triterpenes liposoluble constituent, the more complete and relative amount raising of total active constituent content helps the application of various preparations.Preparation method of the present invention need not heating, energy savings, extraction ratio height.
The specific embodiment
Embodiment one.
The Callicarpa nudiflora medical material is from Hainan, after measured ursolic acid content 0.21%, verbascoside content 0.32%.Get and pulverize medical material 100g, soak 60 min with 80% ethanol 800ml.Under ultrasonic frequency 40kHz, extract 40min then, filter.Filtering residue adds 80% ethanol 400ml again and soaks 60min, under ultrasonic frequency 40kHz, repeats to extract 20min, filters and merges filtrate twice, and the ethanol that reclaims in the filtrate gets ethanol extract extractum.
The filtering residue that above-mentioned ethanol extraction is crossed is a solvent with 1000ml water again, under ultrasonic frequency 40kHz, extracts 40min, and after-filtration, aqueous extract get water extract extractum behind concentrating under reduced pressure.
With two kinds of extractum merging, mixing, 0.85Mpa, 60 ℃ are concentrated in vacuo to thick paste.Above thick paste is at 0.85MPa, and 60 ℃ of vacuum dryings arrive water content below 5%.The extractum yield is 18.7%, is crushed to 80 orders, gets Callicarpa nudiflora extract.
The every sanitary index of extract meets the WM2-2001 " medicinal plants and preparation are imported and exported green industry standard " that State Ministry of Foreign Trade and Economic Cooperation issues.Measure through the HPLC method, wherein ursolic acid content 0.92%; Verbascoside content is 1.37%.
Embodiment two.
The Callicarpa nudiflora medical material is from Hainan, after measured ursolic acid content 0.21%, verbascoside content 0.32%.Get and pulverize medical material 100g, soak 90 min with 70% ethanol 700ml.Under ultrasonic frequency 40kHz, extract 30min then, filter.Filtering residue adds 70% ethanol 300ml again and soaks 90min, under ultrasonic frequency 40kHz, repeats to extract 15min, filters and merges filtrate twice, and the ethanol that reclaims in the filtrate gets ethanol extract extractum.
The filtering residue that above-mentioned ethanol extraction is crossed is a solvent with 1200ml water again, under ultrasonic frequency 40kHz, extracts 50min, and after-filtration, aqueous extract get water extract extractum behind concentrating under reduced pressure.
With two kinds of extractum merging, mixing, 0.85Mpa, 60 ℃ are concentrated in vacuo to thick paste.Above thick paste is at 0.85MPa, and 60 ℃ of vacuum dryings arrive water content below 5%.The extractum yield is 19.8%, gets Callicarpa nudiflora extract.
Embodiment three.
The Callicarpa nudiflora medical material is from Hainan, after measured ursolic acid content 0.21%, verbascoside content 0.32%.Get and pulverize medical material 100g, soak 70 min with 90% ethanol 700ml.Under ultrasonic frequency 40kHz, extract 30min then, filter.Filtering residue adds 90% ethanol 400ml again and soaks 70min, under ultrasonic frequency 40kHz, repeats to extract 25min, filters and merges filtrate twice, and the ethanol that reclaims in the filtrate gets ethanol extract extractum.
The filtering residue that above-mentioned ethanol extraction is crossed is a solvent with 800ml water again, under ultrasonic frequency 40kHz, extracts 30min, and after-filtration, aqueous extract get water extract extractum behind concentrating under reduced pressure.
With two kinds of extractum merging, mixing, 0.85Mpa, 60 ℃ are concentrated in vacuo to thick paste.Above thick paste is at 0.85MPa, and 60 ℃ of vacuum dryings arrive water content below 5%.The extractum yield is 19.2%, gets Callicarpa nudiflora extract.
Embodiment four: the granule preparation.
[method for making] gets the Callicarpa nudiflora extract 120g by example of the present invention one preparation, adds cane sugar powder, dextrin is an amount of, and mixing is made granule with 60% ethanol, and drying is made the 1000g granule, promptly.
[assay] ursolic acid content is measured: high performance liquid chromatography records every bag of Callicarpa nudiflora granule (3g/ bag) ursolic acid content and is no less than 2.6 mg.
Contain the verbascoside content assaying method: high performance liquid chromatography records every bag of Callicarpa nudiflora granule (3g/ bag) and contains verbascoside content and be no less than 4.2mg.
Embodiment five: preparation tablets.
[method for making] gets the Callicarpa nudiflora extract 120g by example of the present invention one preparation, and adding appropriate amount of auxiliary materials, to make its total amount be 500g, granulate, and oven dry, granulate, tabletting, sugar coating is made 1000, promptly.
[specification] every 0.5g.
[assay] ursolic acid content is measured: high performance liquid chromatography records and contains fruit acid content in per 3 of the Callicarpa nudiflora sheet and be no less than 2.5 mg.
Contain the verbascoside content assaying method: high performance liquid chromatography records and contains stamen flower glucosides content in per 3 of the Callicarpa nudiflora tablet and be no less than 3.9mg.
Embodiment six: the capsule preparation.
[method for making] gets the Callicarpa nudiflora extract 120g by example one preparation of the present invention, adds starch 160g, and mixing is made granule with 60% ethanol, and drying adds magnesium stearate 2g, and mixing, filled capsules are promptly.
[specification] every 0.3g.
[assay] ursolic acid content is measured: high performance liquid chromatography records and contains ursolic acid content in per 2 of the Callicarpa nudiflora sheet and be no less than 2.0 mg.
The verbascoside content assaying method: high performance liquid chromatography records and contains verbascoside in per 2 of the Callicarpa nudiflora capsule and be no less than 3.1mg.
Embodiment seven: the oral liquid preparation.
[method for making] gets the Callicarpa nudiflora extract 60g by example one preparation of the present invention, add pure water 1500ml, add an amount of natural sweetener, HPCD, cosolvent, xanthan gum, heated and stirred 30 minutes, 60 order nylon cloths filter, put coldly, drip proper amount of edible essence mixing, adding clean water, to make total measurement (volume) to 500ml be 2000ml.Fill (10ml), sterilization are promptly.
[specification] every bottle of 10ml.
[assay] ursolic acid content is measured: high performance liquid chromatography records and contains ursolic acid content in every bottle of the Callicarpa nudiflora oral liquid and be no less than 1.98mg.
The verbascoside content assaying method: high performance liquid chromatography records and contains stamen flower glucosides content in every bottle of the Callicarpa nudiflora oral liquid and be no less than 3.1mg.
Claims (4)
1. a Callicarpa nudiflora extract comprises flavone compound, water soluble ingredient, it is characterized in that: also include diterpene, triterpenes liposoluble constituent.
2. a kind of Callicarpa nudiflora extract according to claim 1 is characterized in that: described diterpene, triterpenes liposoluble constituent comprise a kind of in pier fruit acid, the ursolic acid at least; Flavone compound comprises a kind of in luteolin, luteolin glycosides, the verbascoside at least.
3. the preparation method of the described a kind of Callicarpa nudiflora extract of claim 1 is characterized in that: may further comprise the steps:
1) Callicarpa nudiflora is pulverized medical material doubly to measure concentration with 7-9 is 70-90% soak with ethanol 60-90min, 30-50min is extracted with the ultrasonic extraction device in the back, filter then, filtering residue adds 3-5 again, and doubly to measure concentration be 70-90% soak with ethanol 60-90min, 15-25min is extracted with the ultrasonic extraction device in the back, filtration also merges filtrate twice, and 1. the ethanol that reclaims in the filtrate get extractum;
2) filtering residue crossed of above-mentioned ethanol extraction is a solvent with 8-12 times of water gaging again, extracts 30-50min with the ultrasonic extraction device, filter afterwards, aqueous extract behind concentrating under reduced pressure extractum 2.;
3) merge extractum 1. with extractum 2., be condensed into thick paste under the vacuum, with thick paste dry to moisture below 5%, Callicarpa nudiflora extract.
4. the described a kind of Callicarpa nudiflora extract of claim 1 is characterized in that: described extract is used to prepare antibacterial, antiinflammatory, hemostasis, analgesia and astringent medicine.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102697866A (en) * | 2012-06-26 | 2012-10-03 | 南京同仁堂药业有限责任公司 | Ultrasonic extraction process for particles for removing urinary calculus |
| CN103272260A (en) * | 2013-06-13 | 2013-09-04 | 海南医学院 | Chitosan composite medical dressing comprising callicarpa nudiflora extract and preparation method thereof |
| CN104262307A (en) * | 2014-08-22 | 2015-01-07 | 海南医学院 | 3,4-open-ring helianthemum diterpenoid type compounds, preparing method thereof and applications of the compounds |
| CN104530147A (en) * | 2014-11-27 | 2015-04-22 | 普正药业股份有限公司 | Method for preparing verbascoside standard product from callicarpa nudiflora leaf |
| CN104644882A (en) * | 2015-01-05 | 2015-05-27 | 海南医学院 | Callicarpa nudiflora extract containing phenylethanoid glycoside and preparation method thereof |
| CN104693312A (en) * | 2015-02-06 | 2015-06-10 | 南昌航空大学 | Method for simultaneously extracting various effective constituents from callicarpa cathayana and application thereof |
| CN106266262A (en) * | 2015-06-05 | 2017-01-04 | 九芝堂股份有限公司 | A kind of Callicarpa nudiflora extract with antiinflammatory action |
| CN107998222A (en) * | 2017-12-07 | 2018-05-08 | 海南大学 | Beautyberry extract, its preparation method and application |
| CN111557986A (en) * | 2020-06-11 | 2020-08-21 | 江西普正制药股份有限公司 | Callicarpa nudiflora extract and application thereof in preparation of medicine for treating allergic purpura |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102697866A (en) * | 2012-06-26 | 2012-10-03 | 南京同仁堂药业有限责任公司 | Ultrasonic extraction process for particles for removing urinary calculus |
| CN103272260A (en) * | 2013-06-13 | 2013-09-04 | 海南医学院 | Chitosan composite medical dressing comprising callicarpa nudiflora extract and preparation method thereof |
| CN104262307B (en) * | 2014-08-22 | 2017-04-12 | 海南医学院 | 3,4-open-ring helianthemum diterpenoid type compounds, preparing method thereof and applications of the compounds |
| CN104262307A (en) * | 2014-08-22 | 2015-01-07 | 海南医学院 | 3,4-open-ring helianthemum diterpenoid type compounds, preparing method thereof and applications of the compounds |
| CN104530147A (en) * | 2014-11-27 | 2015-04-22 | 普正药业股份有限公司 | Method for preparing verbascoside standard product from callicarpa nudiflora leaf |
| CN104530147B (en) * | 2014-11-27 | 2016-02-24 | 普正药业股份有限公司 | A kind of extraction from callicarpa nudiflora leaf prepares the method for verbascoside standard substance |
| CN104644882A (en) * | 2015-01-05 | 2015-05-27 | 海南医学院 | Callicarpa nudiflora extract containing phenylethanoid glycoside and preparation method thereof |
| CN104693312A (en) * | 2015-02-06 | 2015-06-10 | 南昌航空大学 | Method for simultaneously extracting various effective constituents from callicarpa cathayana and application thereof |
| CN104693312B (en) * | 2015-02-06 | 2017-01-04 | 南昌航空大学 | Method that in Folium Callicarpae Formosanae, plurality of active ingredients is extracted simultaneously and application |
| CN106266262A (en) * | 2015-06-05 | 2017-01-04 | 九芝堂股份有限公司 | A kind of Callicarpa nudiflora extract with antiinflammatory action |
| CN107998222A (en) * | 2017-12-07 | 2018-05-08 | 海南大学 | Beautyberry extract, its preparation method and application |
| CN111557986A (en) * | 2020-06-11 | 2020-08-21 | 江西普正制药股份有限公司 | Callicarpa nudiflora extract and application thereof in preparation of medicine for treating allergic purpura |
| CN111557986B (en) * | 2020-06-11 | 2022-01-07 | 江西普正制药股份有限公司 | Callicarpa nudiflora extract and application thereof in preparation of medicine for treating allergic purpura |
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Denomination of invention: Callicarpa nudiflora Hook. et Arn. extract, preparation method and application thereof Effective date of registration: 20200317 Granted publication date: 20130501 Pledgee: Jizhou sub branch of Jiujiang Bank Co.,Ltd. Pledgor: Jiangxi Puzheng Pharmaceutical Co.,Ltd. Registration number: Y2020980000760 |
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