CN103450213A - Method for extracting Indian epimeredi herb dilactone from Indian epimeredi herb leaves - Google Patents
Method for extracting Indian epimeredi herb dilactone from Indian epimeredi herb leaves Download PDFInfo
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- CN103450213A CN103450213A CN 201310410004 CN201310410004A CN103450213A CN 103450213 A CN103450213 A CN 103450213A CN 201310410004 CN201310410004 CN 201310410004 CN 201310410004 A CN201310410004 A CN 201310410004A CN 103450213 A CN103450213 A CN 103450213A
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Abstract
The invention relates to a method for extracting Indian epimeredi herb dilactone from Indian epimeredi herb leaves, which comprises the following steps: 1) performing ultrahigh-pressure extraction on the Indian epimeredi herb leaves by use of an alcohol solution, combining the extract liquid and recovering a solvent to obtain an extract of the Indian epimeredi herb leaves; 2) performing magnesium oxide column chromatography on the extract, performing gradient elution by use of petroleum ether-ethyl acetate, collecting the target eluent and concentrating and drying to obtain a crude extract; 3) performing chromatographic separation on the crude product to obtain Indian epimeredi herb dilactone. The method for extracting Indian epimeredi herb dilactone, provided by the invention, has the advantage that abundant Indian epimeredi herb dilactone can be effectively extracted from the Indian epimeredi herb dilactone leaves so as to provide abundant Indian epimeredi herb dilactone for large-scale preparation of medicines taking Indian epimeredi herb dilactone as a main active ingredient.
Description
Technical field
The invention belongs to the traditional Chinese medicine extraction separation technology field, relate to a kind of method for preparing the parsnip dilactone of separating from windproof blade of grass.
Background technology
Parsnip dilactone (Ovatodiolide), molecular formula is C20H24O4, and molecular weight is 328.41, and structural formula is
The parsnip dilactone derives from the leaf of Labiatae (Labiatae) parsnip Anisomeles indica (L.) O.Ktze..The parsnip dilactone has cytotoxic activity, to the IC50 of KB cell, is 0.6 μ g/mL; There is hypotensive effect, suppress contraction and the Ca of isolated frog heart
2+stream, cause the hypotensive effect that dog is of short duration, but do not suppress Zinc metallopeptidase Zace1 (ACE).Suppress myocardial contraction, tangerine anticalcium ionic current.
At present, there is not yet preparation method's Patents report of high-content parsnip dilactone.
Summary of the invention
The purpose of this invention is to provide a kind of method of extracting the parsnip dilactone from windproof blade of grass.
The objective of the invention is to be achieved through the following technical solutions:
A kind of method of extracting the parsnip dilactone from windproof blade of grass is characterized in that comprising the following steps:
1) get dry windproof blade of grass, through pulverization process, controlling the medicinal material particle diameter is 40 orders, adds and uses ethanolic soln, adopts the superelevation platen press to be extracted, united extraction liquid, and concentration and recovery ethanol, obtain medicinal extract;
2) on above-mentioned medicinal extract, magnesium oxide is lived, and the petroleum ether-ethyl acetate gradient elution is collected the target elutriant, and concentrate drying obtains crude extract;
3) above-mentioned crude extract is carried out to chromatographic separation, obtain the parsnip dilactone.
According to the method further comprising the steps 4 of extracting the parsnip dilactone from windproof blade of grass of the present invention): the elutriant that contains the parsnip dilactone is carried out to recrystallization.This step is specific as follows carries out: the elutriant of the parsnip dilactone obtained combining step 3), carry out recrystallization with acetone again after evaporate to dryness, thereby obtain parsnip dilactone colourless crystallization.
In described step 1), ethanolic soln is the 80-90% aqueous ethanolic solution.
In described step 1), the solid-liquid volume ratio is 1:12-1:18.
In described step 1), ultra-high voltage extraction pressure is 300-600MPa, and temperature is 35-55 ℃, and dwell time 5-10min, repeat release 2-3 time of boosting.
Described step 2) in, magnesium oxide is neutral magnesium oxide, and the order number is the 100-200 order, and post is pressed as 5-7.5bar, and the post blade diameter length ratio is 1:10-12.
Described step 2) PetroChina Company Limited.'s ether-ethyl acetate volume ratio is 13:1-1:1.
In described step 3), chromatographic separation adopts high speed adverse current chromatogram to carry out, and its two-phase solvent system is normal hexane-ethyl acetate-methanol-water, and volume ratio is 5:7:5:3, and the high-speed counter-current chromatograph rotating speed is 900-1050rpm, and flow rate of mobile phase is 3.5-5ml/min.
The positively effect of present method is:
(1) present method adopts the superelevation platen press to extract, and solvent consumption is few, and consuming time short, yield is high, and can not destroy the biological activity of effective constituent;
(2) use sherwood oil, ethyl acetate, acetone etc. in the column chromatography process, alternative common chloroform used, methyl alcohol etc., safety non-toxic, environmental protection;
(3) adopt high-speed countercurrent chromatography, yield is high, preparation amount is large, preparation cycle is short;
(4) the processing step operation is simpler, easy to operate, can carry out scale operation, and products obtained therefrom purity is high.
Further illustrate the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment
Embodiment 1:
Get dry windproof blade of grass, through pulverization process, controlling particle diameter is 40 orders, takes 200g, add 15 times of 80% ethanolic soln, adopt the superelevation platen press to be extracted, extraction pressure is 400MPa, and temperature is 35 ℃, dwell time 5min, release 2 times that repeat to boost, united extraction liquid, concentrating under reduced pressure, carry out column chromatography, chromatography column be take neutral magnesium oxide as filler, and granularity is 100 orders, and post is pressed as 5bar, the post blade diameter length ratio is 1:10, petroleum ether-ethyl acetate 12:1,5:1,1:1 gradient elution, collect the target elutriant, and concentrate drying obtains crude extract, adopt the parsnip dilactone in high-speed countercurrent chromatography separation and purification crude extract, take volume ratio 5:7:5:3 normal hexane-ethyl acetate-methanol-water as the two-phase solvent system, the upper high speed adverse current chromatogram post of filling with mutually is stationary phase, rotate main frame, the high-speed counter-current chromatograph rotating speed is 1000rpm, pump into the lower moving phase of doing mutually, flow rate of mobile phase is 4ml/min, moving phase is dissolved crude extract by the sampling valve sample introduction, the UV-detector on-line monitoring, the detection wavelength is 208nm, collect parsnip dilactone component, carry out vacuum concentration, carry out recrystallization with acetone again after evaporate to dryness, obtain parsnip dilactone colourless crystallization, content 96.7%.
Embodiment 2:
Get dry windproof blade of grass, through pulverization process, controlling particle diameter is 40 orders, takes 500g, add 12 times of 90% ethanolic soln, adopt the superelevation platen press to be extracted, extraction pressure is 300MPa, and temperature is 45 ℃, dwell time 10min, release 2 times that repeat to boost, united extraction liquid, concentrating under reduced pressure, carry out column chromatography, chromatography column be take neutral magnesium oxide as filler, and granularity is 100 orders, and post is pressed as 6bar, the post blade diameter length ratio is 1:10, petroleum ether-ethyl acetate 12:1,5:1,1:1 gradient elution, collect the target elutriant, and concentrate drying obtains crude extract, adopt the parsnip dilactone in high-speed countercurrent chromatography separation and purification crude extract, take volume ratio 5:7:5:3 normal hexane-ethyl acetate-methanol-water as the two-phase solvent system, the upper high speed adverse current chromatogram post of filling with mutually is stationary phase, rotate main frame, the high-speed counter-current chromatograph rotating speed is 950rpm, pump into the lower moving phase of doing mutually, flow rate of mobile phase is 3.5ml/min, moving phase is dissolved crude extract by the sampling valve sample introduction, the UV-detector on-line monitoring, the detection wavelength is 208nm, collect parsnip dilactone component, carry out vacuum concentration, carry out recrystallization with acetone again after evaporate to dryness, obtain parsnip dilactone colourless crystallization, content 97.7%.
Embodiment 3:
Get dry windproof blade of grass, through pulverization process, controlling particle diameter is 40 orders, takes 500g, add 15 times of 90% ethanolic soln, adopt the superelevation platen press to be extracted, extraction pressure is 400MPa, and temperature is 40 ℃, dwell time 8min, release 3 times that repeat to boost, united extraction liquid, concentrating under reduced pressure, carry out column chromatography, chromatography column be take neutral magnesium oxide as filler, and granularity is 100 orders, and post is pressed as 7.5bar, the post blade diameter length ratio is 1:12, petroleum ether-ethyl acetate 11:1,4:1,1:1 gradient elution, collect the target elutriant, and concentrate drying obtains crude extract, adopt the parsnip dilactone in high-speed countercurrent chromatography separation and purification crude extract, take volume ratio 5:7:5:3 normal hexane-ethyl acetate-methanol-water as the two-phase solvent system, the upper high speed adverse current chromatogram post of filling with mutually is stationary phase, rotate main frame, the high-speed counter-current chromatograph rotating speed is 900rpm, pump into the lower moving phase of doing mutually, flow rate of mobile phase is 4ml/min, moving phase is dissolved crude extract by the sampling valve sample introduction, the UV-detector on-line monitoring, the detection wavelength is 208nm, collect parsnip dilactone component, carry out vacuum concentration, carry out recrystallization with acetone again after evaporate to dryness, obtain parsnip dilactone colourless crystallization, content 97.1%.
Embodiment 4:
Get dry windproof blade of grass, through pulverization process, controlling particle diameter is 40 orders, takes 500g, add 18 times of 80% ethanolic soln, adopt the superelevation platen press to be extracted, extraction pressure is 600MPa, and temperature is 55 ℃, dwell time 5min, release 2 times that repeat to boost, united extraction liquid, concentrating under reduced pressure, carry out column chromatography, chromatography column be take neutral magnesium oxide as filler, and granularity is 100 orders, and post is pressed as 7bar, the post blade diameter length ratio is 1:12, petroleum ether-ethyl acetate 11:1,4:1,1:1 gradient elution, collect the target elutriant, and concentrate drying obtains crude extract, adopt the parsnip dilactone in high-speed countercurrent chromatography separation and purification crude extract, take volume ratio 5:7:5:3 normal hexane-ethyl acetate-methanol-water as the two-phase solvent system, the upper high speed adverse current chromatogram post of filling with mutually is stationary phase, rotate main frame, the high-speed counter-current chromatograph rotating speed is 950rpm, pump into the lower moving phase of doing mutually, flow rate of mobile phase is 3.5ml/min, moving phase is dissolved crude extract by the sampling valve sample introduction, the UV-detector on-line monitoring, the detection wavelength is 208nm, collect parsnip dilactone component, carry out vacuum concentration, carry out recrystallization with acetone again after evaporate to dryness, obtain parsnip dilactone colourless crystallization, content 97.3%.
Embodiment 5:
Get dry windproof blade of grass, through pulverization process, controlling particle diameter is 40 orders, takes 1kg, add 18 times of 85% ethanolic soln, adopt the superelevation platen press to be extracted, extraction pressure is 600MPa, and temperature is 40 ℃, dwell time 7min, release 3 times that repeat to boost, united extraction liquid, concentrating under reduced pressure, carry out column chromatography, chromatography column be take neutral magnesium oxide as filler, and granularity is 100 orders, and post is pressed as 6bar, the post blade diameter length ratio is 1:10, petroleum ether-ethyl acetate 13:1,5:1,1:1 gradient elution, collect the target elutriant, and concentrate drying obtains crude extract, adopt the parsnip dilactone in high-speed countercurrent chromatography separation and purification crude extract, take volume ratio 5:7:5:3 normal hexane-ethyl acetate-methanol-water as the two-phase solvent system, the upper high speed adverse current chromatogram post of filling with mutually is stationary phase, rotate main frame, the high-speed counter-current chromatograph rotating speed is 1050rpm, pump into the lower moving phase of doing mutually, flow rate of mobile phase is 5ml/min, moving phase is dissolved crude extract by the sampling valve sample introduction, the UV-detector on-line monitoring, the detection wavelength is 208nm, collect parsnip dilactone component, carry out vacuum concentration, carry out recrystallization with acetone again after evaporate to dryness, obtain parsnip dilactone colourless crystallization, content 97.5%.
Claims (10)
1. a method of extracting the parsnip dilactone from windproof blade of grass is characterized in that comprising the following steps:
1) get dry windproof blade of grass, through pulverization process, controlling the medicinal material particle diameter is 40 orders, adds and uses ethanolic soln, adopts the superelevation platen press to be extracted, united extraction liquid, and concentration and recovery ethanol, obtain medicinal extract;
2) on above-mentioned medicinal extract, magnesium oxide is lived, and the petroleum ether-ethyl acetate gradient elution is collected the target elutriant, and concentrate drying obtains crude extract;
3) above-mentioned crude extract is carried out to chromatographic separation, obtain the parsnip dilactone.
2. the method for extracting the parsnip dilactone from windproof blade of grass according to claim 1, it is characterized in that: the method comprises the following steps 4): the elutriant that contains the parsnip dilactone is carried out to recrystallization.
3. the method for extracting the parsnip dilactone from windproof blade of grass according to claim 1, it is characterized in that: in described step 1), ethanolic soln is the 80-90% aqueous ethanolic solution.
4. according to the described method of extracting the parsnip dilactone from windproof blade of grass of any one in claims 1 to 3, it is characterized in that: in described step 1), the solid-liquid volume ratio is 1:12-1:18.
5. according to the described method of extracting the parsnip dilactone from windproof blade of grass of any one in claims 1 to 3, it is characterized in that: in described step 1), ultra-high voltage extraction pressure is 300-600MPa, temperature is 35-55 ℃, and dwell time 5-10min, repeat release 2-3 time of boosting.
6. according to the described method of extracting the parsnip dilactone from windproof blade of grass of any one in claims 1 to 3, it is characterized in that: described step 2), magnesium oxide is neutral magnesium oxide, the order number is the 100-200 order, and post is pressed as 5-7.5bar, and the post blade diameter length ratio is 1:10-12.
7. according to the described method of extracting the parsnip dilactone from windproof blade of grass of any one in claims 1 to 3, it is characterized in that: described step 2) PetroChina Company Limited.'s ether-ethyl acetate volume ratio is 13:1-1:1.
8. according to the described method of extracting the parsnip dilactone from windproof blade of grass of any one in claims 1 to 3, it is characterized in that: in described step 3), chromatographic separation adopts high speed adverse current chromatogram to carry out, its two-phase solvent system is normal hexane-ethyl acetate-methanol-water, and volume ratio is 5:7:5:3.
9. the method for extracting the parsnip dilactone from windproof blade of grass according to claim 8, it is characterized in that: described high-speed counter-current chromatograph rotating speed is 900-1050rpm, flow rate of mobile phase is 3.5-5ml/min.
10. the method for extracting the parsnip dilactone from windproof blade of grass according to claim 3, it is characterized in that: described step 4) is carried out as follows: the elutriant of the parsnip dilactone obtained combining step 3), carry out recrystallization with acetone again after evaporate to dryness, thereby obtain parsnip dilactone colourless crystallization.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111303178A (en) * | 2018-12-11 | 2020-06-19 | 天津尚德药缘科技股份有限公司 | Ovatodiolide derivative and salt thereof, preparation method and application thereof in preparing anti-cancer drugs |
| CN112964704A (en) * | 2021-02-04 | 2021-06-15 | 甘肃安卓幸制药有限公司 | Saposhnikovia divaricata lactone detection test paper, colorimetric card and rapid detection method |
| CN113248515A (en) * | 2021-05-08 | 2021-08-13 | 甘肃安卓幸制药有限公司 | Extraction method of saposhnikovia divaricata lactone and saposhnikovia divaricata lactone acid |
-
2013
- 2013-09-11 CN CN 201310410004 patent/CN103450213A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111303178A (en) * | 2018-12-11 | 2020-06-19 | 天津尚德药缘科技股份有限公司 | Ovatodiolide derivative and salt thereof, preparation method and application thereof in preparing anti-cancer drugs |
| CN111303178B (en) * | 2018-12-11 | 2023-01-13 | 合肥尚德药缘生物科技有限公司 | Ovatodiolide derivative and salt thereof, preparation method and application thereof in preparing anti-cancer drugs |
| CN112964704A (en) * | 2021-02-04 | 2021-06-15 | 甘肃安卓幸制药有限公司 | Saposhnikovia divaricata lactone detection test paper, colorimetric card and rapid detection method |
| CN112964704B (en) * | 2021-02-04 | 2024-03-22 | 甘肃润达药业有限公司 | Ledebouriella lactone detection test paper, color chart and rapid detection method |
| CN113248515A (en) * | 2021-05-08 | 2021-08-13 | 甘肃安卓幸制药有限公司 | Extraction method of saposhnikovia divaricata lactone and saposhnikovia divaricata lactone acid |
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Application publication date: 20131218 |