CN1283634C - Felt wort extract, its preparation method and use - Google Patents
Felt wort extract, its preparation method and use Download PDFInfo
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- CN1283634C CN1283634C CN 200410084646 CN200410084646A CN1283634C CN 1283634 C CN1283634 C CN 1283634C CN 200410084646 CN200410084646 CN 200410084646 CN 200410084646 A CN200410084646 A CN 200410084646A CN 1283634 C CN1283634 C CN 1283634C
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- coleus forskohlii
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Abstract
The present invention belongs to the pharmaceutical field of traditional Chinese medicines, particularly to the coleus forskohlii root extract of traditional Chinese medicines, a preparation method thereof and purposes that the coleus forskohlii root extract is used for preparing medicines for preventing and treating asthma and bronchitis. In the present invention, after being pulverized, the whole herb or the root of the coleus forskohlii root is extracted by water-bearing alcohol; after extracting liquid adopts macroporous resin for purification, extract is obtained, and the content of isoforskolin of main active components of the extract is more than 8%. According to animal experiment, the coleus forskohlii root extract of the present invention can obviously suppress the contraction of guinea pig trachea strips of histamine induction separate bodies, and the coleus forskohlii root extract of traditional Chinese medicines is suitable for preparing medicines for preventing and treating asthma and bronchitis.
Description
Technical field:
The invention belongs to field of traditional Chinese medicine pharmacy, relate to Chinese medicine Coleus forskohlii extract and preparation method thereof and Coleus forskohlii extract is used to prepare the purposes of preventing and treating asthma and bronchitis medicine.
Background technology:
Coleus forskohlii Briq. Coleus forskohlii Brig is a Labiatae Coleus plant, have relieving asthma, effect such as cardiac stimulant, step-down, antithrombotic, reduction intraocular pressure, and powerful adenylate cyclase activating effect is arranged.Its effective constituent is mainly laudanum alkane (labdane) type diterpene compound, comprises Floex Kelin (forskolin), isofloex Kelin (isoforskolin) and other analogue.This plant main product is in India and Yunnan Province of China province and other places, and India's product Coleus forskohlii Briq. mainly contains the Floex Kelin according to the literature, and content is 0.1%, and the content of product kind isofloex Kelin, Yunnan is higher, is 0.005%～0.014%.In recent years, Yunnan Province develops the compound granules made from the Yunnan product Coleus forskohlii Briq. compatibility root of purple-flowered peucedanum, Radix Glycyrrhizae, is used for the treatment of asthma and bronchitis, and curative effect is better.The bibliographical information Coleus forskohlii extract has the activity that suppresses the guinea-pig tracheal strip contraction.Relevant prior art has 1. publication number CN 1154861A; 2. publication number CN 1539493A wherein relates to the purifying technique of Coleus forskohlii Briq. efficient part, one, adopt the silicagel column removal of impurities and with chloroform or dichloromethane extraction, be unsuitable for the big production of industry, another process using supercritical fluid extraction needs special equipment; 3. unming Medical College's journal, 2003, (3): 3～4.
Summary of the invention:
The purpose of this invention is to provide a kind of Coleus forskohlii extract that contains formula (1) and preparation method thereof, present method economy, easy and be applicable to industrialized production.Another object of the present invention provides this extract is used to prepare the purposes of preventing and treating asthma and bronchitis medicine.
Coleus forskohlii extract of the present invention prepares by following method:
After Coleus forskohlii Briq. herb or root pulverizing, extract with aqueous ethanol, extracting solution concentrates the back and adds flocculation agent, leave standstill the centrifugal or filtration in back, or directly centrifugal or filtration, get centrifuged supernatant or filtrate and carry out macroporous resin adsorption, impurity is removed in the lower alcohol aqueous solution drip washing that water and concentration are lower successively, use the higher lower alcohol wash-out of concentration again, elutriant be concentrated into do or remove spraying drying behind the lower alcohol, Coleus forskohlii extract of the present invention.This extract can be further with organic solvent extraction purifying such as ethyl acetate.
Coleus forskohlii Briq. herb or the root pulverized are carried with 20～95% ethanol heat, and the solvent consumption is about 4～8 times of crude drug amount first; Or with 20～95% ethanol percolate extraction, the solvent consumption is about 4～12 times of crude drug amount; Extracting solution concentrates the back and adds flocculation agent (quiet as 1% coacervation), leave standstill behind the certain hour centrifugal or filter, or concentrated solution is directly centrifugal or filtration, (macroporous resin is a polystyrene type porousness polymeric adsorbent with carrying out macroporous resin adsorption after centrifuged supernatant or the filtrate adjusting pH value, as D101, ZTC-1, AB-8, SIP1300, HP20 type macroporous resin etc.), impurity is removed in the lower alcohol aqueous solution drip washing that water and concentration are lower successively, and lower alcohol is C such as methyl alcohol, ethanol or propyl alcohol
1～C
5Alcohols, its concentration are 5～50%, use the higher lower alcohol wash-out of concentration again, and the concentration of lower alcohol is 50～95%, elutriant is concentrated into does or remove spraying drying behind the ethanol, Coleus forskohlii extract of the present invention, yield is 0.1%; This extract is further used ethyl acetate extraction, divides and to get ethyl acetate layer, be concentrated into dried, solid substance, yield is 0.03%.
Mainly contain the isofloex Kelin in the Coleus forskohlii extract of above-mentioned acquisition and the ethyl acetate extraction gained solid substance thereof, have the chemical structure of following formula (1).
The HPLC quantitative analysis results shows that the content of isofloex Kelin in Coleus forskohlii extract and ethyl acetate extraction gained solid substance thereof is respectively more than 8% with more than 20%.
Macroporous resin of the present invention is a polystyrene type porousness polymeric adsorbent, and before last macroporous resin, centrifuged supernatant or pH value of filtrate scope are 5～12; Described lower alcohol is C
1～C
5Lower alcohol, its moisture concentration of lower alcohols is 5～50%; Described high-concentration aqueous concentration of lower alcohols is 50～95%.
Carry out biological activity determination by experimentation on animals, detect the influence that stripped guinea pig trachea that Coleus forskohlii extract of the present invention causes histamine is shunk.The result shows that behind the adding histamine, the tracheae sample produces and shrinks, and amplitude is 1573 ± 570mg, and Coleus forskohlii extract makes sample produce obvious diastole, and its maximum diastole is lower than baseline, is-1121 ± 566mg, with solvent marked difference is arranged.The diastole that Coleus forskohlii extract produces is typical S type, calculates its EC with the Bliss method
50Be 4.02ug/ml, the 95% credible 5.28～2.97ug/ml that is limited to, 95% fiducial limit rate is 28.72%.
Coleus forskohlii extract of the present invention and the solid substance that is further purified gained thereof can be used as raw material and make capsule, soft capsule, tablet, dripping pill, injection, oral liquid, aerosol, sprays, powder inhalation and compound preparation according to a conventional method, are used to prevent and treat asthma and bronchitis medicine.
Embodiment:
Providing embodiment below further specifies the present invention but the present invention is not limited.
Embodiment 1
Coleus forskohlii Briq. herb after 100 kilograms of pulverizing, drop into extractor, carry 3 times with 400 liters of heat of 70% ethanol successively at 90～100 ℃, each extraction time is 90 minutes, merge No. 3 times extracting solution, be concentrated into 100 liters, add quiet 5 liters of 1% coacervation, leave standstill 1h, filter, filtrate is adjusted to pH=8 and with distilled water diluting to 400 liter, flow velocity with 2BV/h (BV is the column volume of macroporous resin) passes through 300 liters of SIP1300 type macroporous resin column, remove impurity with 1500 liters of distilled water and 900 liter of 30% ethanol drip washing successively, use 900 liter of 85% ethanol elution again, collect elutriant, be concentrated into dried, get Coleus forskohlii extract of the present invention, heavy 100g is 0.1% by crude drug amount yield.With this extract further with ethyl acetate extraction 2 times, each consumption 1000ml, the combined ethyl acetate layer, be concentrated into dried, solid substance 30g, be 0.03% by crude drug amount yield.
Embodiment 2
Coleus forskohlii Briq. root after 100 kilograms of pulverizing, with diacolation behind 300 liters of immersions of 80% ethanol 24h, collect 600 liters of percolates, be concentrated into 80 liters, filter, filtrate is adjusted to pH=9 and with distilled water diluting to 200 liter, flow velocity with 2BV/h passes through 300 liters of AB-8 type macroporous resin column, remove impurity with 1500 liters of distilled water and 900 liter of 40% ethanol drip washing successively, use 900 liter of 90% ethanol elution again, collect elutriant, be concentrated into dried, get Coleus forskohlii extract of the present invention, heavy 120g is 0.12% by crude drug amount yield.Is that 8 aqueous solution 1000ml disperses with this extract with the pH value, with ethyl acetate extraction 2 times, and each consumption 1000ml, the combined ethyl acetate layer is concentrated into driedly, can get solid substance 40g, is 0.04% by crude drug amount yield.
Embodiment 3
Get cavy, male and female are regardless of, and after the execution, cut skin of neck and muscle, take out tracheae and place nutritive medium.Remove tracheae extraneous tissue on every side, tracheae is cut into the spiral groove of wide about 3mm.Get the tracheae spiral groove that contains 3 sections muscle, place to contain Kreb ' s liquid, an end is fixed, and an end is connected in tonotransducer.Add 2g tension force, 37 ℃, logical 95%O
2+ 5%CO
2Gas mixture is stablized 1h.Adding histamine, to make its final concentration be 1ug/ml, record sample shrinkage amplitude.After treating that it reaches shrinkage peak, add Coleus forskohlii extract of the present invention, the record sample shrinks height behind the effect 3min, adds the Coleus forskohlii extract of next concentration then.Coleus forskohlii extract accumulation final concentration is followed successively by 0.5,1,2,4,6,10,16,20 μ g/ml.Other gets sample, and the PEG that adds respective volume is as blank.
Record adds sample shrinks behind the histamine amplitude, add the maximum diastole amplitude behind Coleus forskohlii extract and the PEG.Sample contraction/relaxation amplitude when measuring different pharmaceutical concentration, to add histamine post shrinkage amplitude is 100% contraction, add behind the Coleus forskohlii extract the maximum diastole amplitude of sample and be 0% and shrink, calculate the percentage that adds sample diastole behind the Coleus forskohlii extract and calculate it by the Bliss method and suppress the EC that histamine causes that tracheae shrinks
50
The exercising result that the table 1 stripped guinea pig trachea that to be Coleus forskohlii extract cause histamine is shunk.
Table 1
Wherein, the * Coleus forskohlii extract is 0% to shrink with maximum diastole, and PEG is 0% to shrink the add-on and corresponding Coleus forskohlii extract group equal-volume of PEG in the blank PEG group of * * with the amplitude before the histamine of giving.
| The concentration of Coleus forskohlii extract 1 (μ g/ml) | The percentage of sample diastole (%) | |
| Coleus forskohlii extract | PEG | |
| O.5 1 2 4 6 10 16 20 | 99.12±6.63 94.65±9.17 82.62±8.12 56.76±9.62 30.18±9.44 11.91±6.53 2.89±1.70 0.00±0.00 | 99.37±5.00 99.04±0.29 97.57±4.24 94.35±6.26 91.23±6.51 84.92±6.90 76.94±5.21 66.21±1.27 |
The result shows that behind the adding histamine, the tracheae sample produces and shrinks, and amplitude is 1573 ± 570mg, and Coleus forskohlii extract makes sample produce obvious diastole, and its maximum diastole is lower than baseline, is-1121 ± 566mg, with solvent marked difference is arranged.The diastole that Coleus forskohlii extract produces is typical S type, calculates its EC with the Bliss method
50Be 4.02ug/ml, the 95% credible 5.28～2.97ug/ml that is limited to, 95% fiducial limit rate is 28.72%.
Claims (4)
1, a kind of preparation method of Coleus forskohlii extract is characterized in that comprising the steps:
(1) extracts
After Coleus forskohlii Briq. herb or root are pulverized,, add flocculation agent after extracting solution concentrates, leave standstill the centrifugal or filtration in back with the aqueous ethanol extraction, or directly centrifugal or filtration, centrifuged supernatant or filtrate for later use got;
(2) absorb-elute
Getting above-mentioned supernatant liquor or filtrate regulates after the pH value is 5～12, carry out macroporous resin adsorption, water and concentration are that impurity is removed in 5～50% lower alcohol aqueous solution drip washing successively, be 50～95% lower alcohol wash-out again with concentration, elutriant is concentrated into does or remove spraying drying behind the lower alcohol, extract;
(3) be further purified
Boil off organic solvent after adopting the ethyl acetate organic solvent extraction, get solid substance.
2, according to the preparation method of the described Coleus forskohlii extract of claim 1, it is characterized in that containing in the described extract that makes the isofloex Kelin of formula (1) chemical structure,
The content of described isofloex Kelin in extract is more than 8%, and the content in its ethyl acetate extraction gained solid substance is more than 20%.
3, the preparation method of Coleus forskohlii extract according to claim 1 is characterized in that wherein said macroporous resin is a polystyrene type porousness polymeric adsorbent.
4, the preparation method of Coleus forskohlii extract according to claim 1 is characterized in that wherein said lower alcohol is C
1～C
5Lower alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410084646 CN1283634C (en) | 2004-11-26 | 2004-11-26 | Felt wort extract, its preparation method and use |
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|---|---|---|---|
| CN 200410084646 CN1283634C (en) | 2004-11-26 | 2004-11-26 | Felt wort extract, its preparation method and use |
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|---|---|
| CN1651423A CN1651423A (en) | 2005-08-10 |
| CN1283634C true CN1283634C (en) | 2006-11-08 |
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| CN 200410084646 Expired - Fee Related CN1283634C (en) | 2004-11-26 | 2004-11-26 | Felt wort extract, its preparation method and use |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101843366B (en) * | 2010-04-29 | 2012-01-04 | 云南省玉溪市溶剂厂有限公司 | Tobacco plasticizer containing isoforskolin and preparation method thereof |
| CN103183658A (en) * | 2011-12-29 | 2013-07-03 | 复旦大学 | Method for extracting effective component of coleus forskohlii |
| CN103720668B (en) * | 2012-10-10 | 2016-06-08 | 华东理工大学 | The tablet of a kind of quick release Isoforskolin |
| CN111569008B (en) * | 2020-05-09 | 2021-10-08 | 昆明医科大学 | A pharmaceutical composition for treating neurodegenerative diseases |
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