CN102659585A - Method for simultaneously preparing coltsfoot flower ketone and new coltsfoot flower lactone - Google Patents
Method for simultaneously preparing coltsfoot flower ketone and new coltsfoot flower lactone Download PDFInfo
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- CN102659585A CN102659585A CN2012101171588A CN201210117158A CN102659585A CN 102659585 A CN102659585 A CN 102659585A CN 2012101171588 A CN2012101171588 A CN 2012101171588A CN 201210117158 A CN201210117158 A CN 201210117158A CN 102659585 A CN102659585 A CN 102659585A
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- China
- Prior art keywords
- ketone
- new
- coltsfoot flower
- tussilagin
- flos farfarae
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Abstract
The invention discloses a method for simultaneously preparing coltsfoot flower ketone and new coltsfoot flower lactone, which comprises the following steps: taking, crushing and alcohol-extracting a bud of a coltsfoot flower, preliminarily separating extracting solution through a column chromatography, purifying by adopting a high-speed counter-current chromatography, placing an eluting solvent system into a liquid separating funnel for layering, taking an upper phase as a fixed phase, taking a lower phase as a mobile phase, taking and dissolving a coltsfoot flower extract into the lower phase, filling a separation column of the fixed phase by using a pump, connecting the head end of the column with a sampling valve, adjusting the flowing speed of the mobile phase and the rotating speed of a main machine, collecting a separation substance in a segmented manner, and concentrating and drying to obtain the coltsfoot flower ketone and the new coltsfoot flower lactone. The separation method has high separation efficiency, and the coltsfoot flower ketone with high content and the new coltsfoot flower lactone with high content can be obtained.
Description
Technical field
The present invention relates to a kind of method for preparing Flos Farfarae ketone and new tussilagin simultaneously, especially relate to a kind of column chromatography combines separation and purification Flos Farfarae ketone and new tussilagin with adverse current chromatogram method.
Background technology
Flos Farfarae ketone and new tussilagin are sesquiterpenoids, derive from the feverfew Flos Farfarae (
Tussilago farfaraL.) bud.Flos Farfarae has nourishing the lung to keep the adverse QI downward, the effect such as only cough of reducing phlegm.Modern pharmacological research shows that Flos Farfarae has cough-relieving to respiratory system, eliminates the phlegm and antiasthmatic effect; Sympathetic nerve, sympathomimetic nerve, vascular smooth muscle etc. had direct excitation; To all being restraining effect at body or stripped gastrointestinal smooth muscle.Flos Farfarae distribution Hebei, Henan, Hubei, Sichuan, Shanxi, Shaanxi, Gansu, the Inner Mongol, Xinjiang, Qinghai, ground such as Tibet, aboundresources.
Flos Farfarae ketone, molecular formula: C
21H
30O
3, molecular weight: 330.47, colourless jelly.New tussilagin, molecular formula: C
21H
28O
4, molecular weight: 344.45..Flos Farfarae ketone and the effect that new tussilagin all has stronger inhibition platelet activation factor can suppress PAF inductive platelet aggregation.
Do not see at present the relevant report of purification Flos Farfarae ketone and new tussilagin as yet.
Summary of the invention
The technical problem that the present invention will solve provides a kind of method of utilizing high-speed countercurrent chromatography purifying Flos Farfarae ketone and new tussilagin.
A kind of method for preparing Flos Farfarae ketone and new tussilagin simultaneously of the present invention is characterized in that following these steps to carrying out:
(1) the withdraw the money bud of coltsfoot is pulverized the back with 80-100% ethanol ultrasonic extraction 1-2 time, and united extraction liquid adding injection class medical active carbon decoloring leaches gac, the extracting solution concentrating under reduced pressure;
(2) liquid concentrator is disperseed with hot water, add 20-100 order silica gel column chromatography, methylene chloride-methanol mixed solvent wash-out, thin layer is followed the tracks of, and collects elutriant, concentrate drying;
(3) adopt high-speed counter-current chromatograph, solvent systems is made up of normal hexane, ETHYLE ACETATE, first alcohol and water, and volume ratio is 6-11:7-15:4-8:3, places separating funnel; On be stationary phase mutually, be moving phase mutually down, get during the dry thing of step (2) is dissolved in time mutually, with pump stationary phase is filled separator column; Main frame is rotated, pump into moving phase, when moving phase flows out, continuous sample introduction; Collect target component according to the detector spectrogram, concentrate, cryodrying promptly gets product.
Amount of activated is the 3-5 ‰ of extracting solution total mass in the said step (1).
The ratio of the mixed solvent that the middle column chromatography of said step (2) is used is 1:3-10.
Said step (3) high speed counter current chromatograph flow rate of mobile phase is controlled at 2-3ml/min, and engine speed is 750-950rpm..
The present invention compared with prior art has following advantage and beneficial effect:
1) the present invention uses the column chromatography enriching and purifying earlier, has reduced the treatment capacity of subsequent handling;
2) adopt the high-speed countercurrent chromatography separation and purification, preparation amount is big, and product purity is high, sample free of losses in the treating processes.
Embodiment
Embodiment 1:
The bud of getting the 10kg Flos Farfarae is pulverized the back with 80% ethanol ultrasonic extraction 2 times, and united extraction liquid adds 3 ‰ injection class medical active carbon decolorings, leaches gac; The extracting solution concentrating under reduced pressure, liquid concentrator disperses with hot water, adds 100 order silica gel column chromatographies; With methylene chloride-methanol (1:3) wash-out; Thin layer is followed the tracks of, and collects elutriant, and concentrate drying gets crude extract;
Get normal hexane, ETHYLE ACETATE, first alcohol and water (6:7:8:3) and place separating funnel, standing demix, on be stationary phase mutually; Descending is moving phase mutually, and sample thief is filled separator column with pump with stationary phase in being dissolved in mutually; Main frame is rotated reach 950rpm, go into moving phase with the 2.0ml/min flow pump, when moving phase flows out; The beginning continuous sample introduction is collected Flos Farfarae ketone flow point and new tussilagin flow point respectively according to the detector spectrogram, concentrates; Cryodrying promptly obtains Flos Farfarae ketone and new tussilagin, and detection level is all more than 98%.
Embodiment 2:
The bud of getting the 10kg Flos Farfarae is pulverized the back with ethanol ultrasonic extraction 1 time, and united extraction liquid adds 5 ‰ injection class medical active carbon decolorings, leaches gac; The extracting solution concentrating under reduced pressure, liquid concentrator disperses with hot water, adds 20 order silica gel column chromatographies; With methylene chloride-methanol (1:10) wash-out; Thin layer is followed the tracks of, and collects elutriant, and concentrate drying gets crude extract;
Get normal hexane, ETHYLE ACETATE, first alcohol and water (11:15:4:3) and place separating funnel, standing demix, on be stationary phase mutually; Descending is moving phase mutually, and sample thief is filled separator column with pump with stationary phase in being dissolved in mutually; Main frame is rotated reach 750rpm, go into moving phase with the 2.0ml/min flow pump, when moving phase flows out; The beginning continuous sample introduction is collected Flos Farfarae ketone flow point and new tussilagin flow point respectively according to the detector spectrogram, concentrates; Cryodrying promptly obtains Flos Farfarae ketone and new tussilagin, and detection level is all more than 98%.
Embodiment 3:
The bud of getting the 10kg Flos Farfarae is pulverized the back with 90% ethanol ultrasonic extraction 2 times, and united extraction liquid adds 4 ‰ injection class medical active carbon decolorings, leaches gac; The extracting solution concentrating under reduced pressure, liquid concentrator disperses with hot water, adds 80 order silica gel column chromatographies; With methylene chloride-methanol (1:5) wash-out; Thin layer is followed the tracks of, and collects elutriant, and concentrate drying gets crude extract;
Get normal hexane, ETHYLE ACETATE, first alcohol and water (7:8:5:3) and place separating funnel, standing demix, on be stationary phase mutually; Descending is moving phase mutually, and sample thief is filled separator column with pump with stationary phase in being dissolved in mutually; Main frame is rotated reach 850rpm, go into moving phase with the 2.5ml/min flow pump, when moving phase flows out; The beginning continuous sample introduction is collected Flos Farfarae ketone flow point and new tussilagin flow point respectively according to the detector spectrogram, concentrates; Cryodrying promptly obtains Flos Farfarae ketone and new tussilagin, and detection level is all more than 98%.
Embodiment 4:
The bud of getting the 10kg Flos Farfarae is pulverized the back with 85% ethanol ultrasonic extraction 2 times, and united extraction liquid adds 5 ‰ injection class medical active carbon decolorings, leaches gac; The extracting solution concentrating under reduced pressure, liquid concentrator disperses with hot water, adds 60 order silica gel column chromatographies; With methylene chloride-methanol (1:5) wash-out; Thin layer is followed the tracks of, and collects elutriant, and concentrate drying gets crude extract;
Get normal hexane, ETHYLE ACETATE, first alcohol and water (9:11:5:3) and place separating funnel, standing demix, on be stationary phase mutually; Descending is moving phase mutually, and sample thief is filled separator column with pump with stationary phase in being dissolved in mutually; Main frame is rotated reach 800rpm, go into moving phase with the 2.8ml/min flow pump, when moving phase flows out; The beginning continuous sample introduction is collected Flos Farfarae ketone flow point and new tussilagin flow point respectively according to the detector spectrogram, concentrates; Cryodrying promptly obtains Flos Farfarae ketone and new tussilagin, and detection level is all more than 98%.
Embodiment 5:
The bud of getting the 10kg Flos Farfarae is pulverized the back with 90% ethanol ultrasonic extraction 2 times, and united extraction liquid adds 4 ‰ injection class medical active carbon decolorings, leaches gac; The extracting solution concentrating under reduced pressure, liquid concentrator disperses with hot water, adds 80 order silica gel column chromatographies; With methylene chloride-methanol (1:8) wash-out; Thin layer is followed the tracks of, and collects elutriant, and concentrate drying gets crude extract;
Get normal hexane, ETHYLE ACETATE, first alcohol and water (10:9:6:3) and place separating funnel, standing demix, on be stationary phase mutually; Descending is moving phase mutually, and sample thief is filled separator column with pump with stationary phase in being dissolved in mutually; Main frame is rotated reach 850rpm, go into moving phase with the 2.0ml/min flow pump, when moving phase flows out; The beginning continuous sample introduction is collected Flos Farfarae ketone flow point and new tussilagin flow point respectively according to the detector spectrogram, concentrates; Cryodrying promptly obtains Flos Farfarae ketone and new tussilagin, and detection level is all more than 98%.
Claims (3)
1. method for preparing Flos Farfarae ketone and new tussilagin simultaneously is characterized in that following these steps to carrying out:
(1) the withdraw the money bud of coltsfoot is pulverized the back with 80-100% ethanol ultrasonic extraction 1-2 time, and united extraction liquid adding injection class medical active carbon decoloring leaches gac, the extracting solution concentrating under reduced pressure;
(2) liquid concentrator is disperseed with hot water, add 20-100 order silica gel column chromatography, methylene chloride-methanol mixed solvent wash-out, thin layer is followed the tracks of, and collects elutriant, concentrate drying;
(3) adopt high-speed counter-current chromatograph, solvent systems is made up of normal hexane, ETHYLE ACETATE, first alcohol and water, and volume ratio is 6-11:7-15:4-8:3, places separating funnel; On be stationary phase mutually, be moving phase mutually down, get during the dry thing of step (2) is dissolved in time mutually, with pump stationary phase is filled separator column; Main frame is rotated, pump into moving phase, when moving phase flows out, continuous sample introduction; Collect target component according to the detector spectrogram, concentrate, cryodrying promptly gets product.
2. the method for preparing Flos Farfarae ketone and new tussilagin simultaneously according to claim 1 is characterized in that amount of activated is the 3-5 ‰ of extracting solution total mass in the said step (1).
3. the method for preparing Flos Farfarae ketone and new tussilagin simultaneously according to claim 1 is characterized in that the ratio of the mixed solvent that the middle column chromatography of said step (2) is used is 1:3-10.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101171588A CN102659585A (en) | 2012-04-20 | 2012-04-20 | Method for simultaneously preparing coltsfoot flower ketone and new coltsfoot flower lactone |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101171588A CN102659585A (en) | 2012-04-20 | 2012-04-20 | Method for simultaneously preparing coltsfoot flower ketone and new coltsfoot flower lactone |
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|---|---|
| CN102659585A true CN102659585A (en) | 2012-09-12 |
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ID=46769198
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|---|---|---|---|
| CN2012101171588A Pending CN102659585A (en) | 2012-04-20 | 2012-04-20 | Method for simultaneously preparing coltsfoot flower ketone and new coltsfoot flower lactone |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103524342A (en) * | 2013-10-24 | 2014-01-22 | 重庆大学 | Method for rapidly separating tussilagone by adopting adjustable ternary solvent system |
| CN103585218A (en) * | 2013-09-30 | 2014-02-19 | 浙江省中药研究所有限公司 | Traditional Chinese medicine drug for treating allergy and preparation method thereof |
| CN103788048A (en) * | 2014-02-27 | 2014-05-14 | 泰山医学院 | Method for ultrasonically extracting total flavones from tussilago farfara |
| CN105732557A (en) * | 2016-04-13 | 2016-07-06 | 山西大学 | Method for separating and extracting 2,2-dimethyl-6-acetyl benzodihydropyrone |
-
2012
- 2012-04-20 CN CN2012101171588A patent/CN102659585A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103585218A (en) * | 2013-09-30 | 2014-02-19 | 浙江省中药研究所有限公司 | Traditional Chinese medicine drug for treating allergy and preparation method thereof |
| CN103524342A (en) * | 2013-10-24 | 2014-01-22 | 重庆大学 | Method for rapidly separating tussilagone by adopting adjustable ternary solvent system |
| CN103524342B (en) * | 2013-10-24 | 2015-09-16 | 重庆大学 | Adopt the method for adjustable ternary solvent system sharp separation tussilagone |
| CN103788048A (en) * | 2014-02-27 | 2014-05-14 | 泰山医学院 | Method for ultrasonically extracting total flavones from tussilago farfara |
| CN105732557A (en) * | 2016-04-13 | 2016-07-06 | 山西大学 | Method for separating and extracting 2,2-dimethyl-6-acetyl benzodihydropyrone |
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Application publication date: 20120912 |