CN102190571A - Extraction method of high purity chalcone from bright moon grass - Google Patents
Extraction method of high purity chalcone from bright moon grass Download PDFInfo
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- CN102190571A CN102190571A CN2010101274250A CN201010127425A CN102190571A CN 102190571 A CN102190571 A CN 102190571A CN 2010101274250 A CN2010101274250 A CN 2010101274250A CN 201010127425 A CN201010127425 A CN 201010127425A CN 102190571 A CN102190571 A CN 102190571A
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Abstract
The invention relates to an extraction method of a chemical substance from bright moon grass, more particularly, to an extraction method of high purity chalcone from bright moon grass. The extraction method of high purity chalcone from the bright moon grass comprises the following steps: step (1), a first extraction process: drying bright moon grass and crushing dried bright moon grass into bright moon grass powder, carrying out the extraction process on the bright moon grass powder with an extraction solvent so as to obtain an extract; step (2), a second extraction process: extracting the extract with an organic solvent to obtain an extract phase and a raffinate phase of the organic solvent; step (3), a separation process: performing vacuum concentration on the extract phase of the organic solvent to obtain a concentrate, separating the concentrate through a column chromatography, followed by elution with an eluant, so as to obtain an effluent containing chalcone, and performing vacuum concentration on the effluent to obtain a chalcone concentrate; and step (4), a crystallization process: crystallizing the chalcone concentrate with an organic solvent to obtain pure chalcone. According the above steps, the chalcone can be extracted from the bright moon grass to obtain the pure chalcone. The extraction method, which has advantages of simple process and low cost, is suitable for industrial production.
Description
Technical field
The invention belongs to medical, chemical field, be specifically related to the extracting method of the chemical substance in the bright moon grass.
Background technology
" bright moon grass ", originate in Japan longevity eight zhang islands, township." bright moon grass " has anti-human senility, thrombus, cancer, and hypoglycemic, blood pressure, cholesterol are improved intestines and stomach or the like function, can treat and prevent 26 kinds of diseases, and be wherein hypoglycemic, the blood pressure effect is the most obvious.Discover that according to Osaka, Japan pharmaceutical university of internal authority mechanism " bright moon grass " contains the germanium higher than genseng, cinnamophenone and multiple natural organic element etc.
Cinnamophenone wherein is anti-oxidant except having, remove the active function of free radical, also have functions such as anti-leishmaniasis (referring to kala-azar especially), anti-inflammatory, anti-HIV, antitumor, antibiotic, immunological enhancement, purposes is very widely arranged in food and medicine industry.
Though contain abundant cinnamophenone in the bright moon grass, also be in initial stage for research China of bright moon grass, be not specifically designed to the method for from the bright moon grass, extracting cinnamophenone at present.From the bright moon grass, extract cinnamophenone as the existing technology of direct employing, complex process, cost height, and be difficult to obtain higher purity.
Summary of the invention
In order to address the above problem, the objective of the invention is to, a kind of extracting method of high purity bright moon grass cinnamophenone is provided, from the bright moon grass, extract cinnamophenone.
Technical problem solved by the invention can realize by the following technical solutions:
The extracting method of high purity bright moon grass cinnamophenone comprises the steps:
(1) extracts, the bright moon grass is dried and crushed into the bright moon grass meal, the bright moon grass meal is extracted with the extraction solvent, obtain extracting solution;
(2) extraction with an organic solvent extracts extracting solution, obtains organic solvent extraction phase and extracting phase;
(3) separate, organic solvent extraction is carried out concentrating under reduced pressure mutually, obtain enriched material, enriched material is passed through column chromatography for separation, the eluent wash-out, acquisition contains the effluent liquid of cinnamophenone, and this effluent liquid of concentrating under reduced pressure, gets the cinnamophenone enriched material;
(4) crystallization promptly gets the pure product of cinnamophenone with the cinnamophenone enriched material with the organic solvent crystallization.
By above-mentioned steps, can from the bright moon grass, cinnamophenone be extracted, obtain the pure product of cinnamophenone, this extracting method technology is simple, with low cost, be suitable for suitability for industrialized production, for the further research of cinnamophenone monomer pharmacology provides raw material.
Step comprises the bright moon grass meal in (1) with the method that the extraction solvent extracts: coldly ooze method, temperature is soaked method or circumfluence method; Described extraction solvent is a kind of in the following solvents: the mixture of A. methyl alcohol and water, and the content of methyl alcohol accounts for 0-100wt% in the mixture; B. the mixture of ethanol and water, alcoholic acid content accounts for 0-100wt% in the mixture; C. the mixture of acetone and water, the content of acetone accounts for 0-100wt% in the mixture;
In the step (2), organic solvent adopts the mode that stirs extraction or adopt Continuous Flow extracting and separating machine to extract to extract and carries extracting solution; Described organic solvent is a kind of in propyl carbinol, ethyl acetate, normal hexane, chloroform or the primary isoamyl alcohol;
In the step (3), when obtaining enriched material, can reclaim organic solvent wherein; Eluent is made up of aqueous ethanolic solution or methanol aqueous solution or aqueous acetone solution, and wherein the ratio that accounts for of water is 100-0wt%, degree of grade or gradient elution; Check effluent liquid with thin-layer chromatography detection method or high performance liquid chromatography, collect the effluent liquid that contains cinnamophenone;
In the step (4), described organic solvent is acetone, ethanol, methyl alcohol, isopropyl ether, chloroform or their mixed solvent.
By to the choosing and, adopt the preparation method of above-mentioned high purity bright moon grass cinnamophenone of each solvent, can from the bright moon grass, extract the pure product of cinnamophenone of higher degree to the optimization of each step.Through experimental verification, the pure product purity of cinnamophenone that obtains by aforesaid method can reach more than 90%.And in the leaching process, adopt reusable column chromatography separation method, and make the nontoxic or recyclable solvents of low toxicity such as water, alcohol, acetone, when having reduced production cost, reduced pollution to environment.
Description of drawings
Fig. 1 is a schematic flow sheet of the present invention.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach purpose and effect is easy to understand, further set forth the present invention below in conjunction with concrete diagram.
The extracting method of high purity bright moon grass cinnamophenone comprises that mainly extract (1), (2) extract, separate (3), four steps of (4) crystallization.The cold method of oozing in the step (1) is extracted with the method for diacolation then at room temperature with the solvent soaking bright moon grass meal of 10～15 times of mass ratioes, and extraction time is 1～5 time.In order to save time, guarantee the extracted amount of cinnamophenone simultaneously, preferred 3 times of extraction time.Temperature in the step (1) soak method under 30～45 ℃ of temperature with solvent soaking bright moon grass meal, the stirring of 5～25 times of mass ratioes and be incubated 3～6 hours; Circumfluence method in the step (1) is the solvent soaking bright moon grass meal with 2～15 times of mass ratioes, and heating makes solvent refluxing and kept reflux state 1～5 hour.The extracting solution vacuum decompression can be concentrated into vacuum tightness before be 0.01～0.1Mpa carrying out step (2), 40～80 ℃ of temperature, and proportion is 1.05～1.15 during 20 ℃ of concentrated solutions; Reclaim the organic solvent in the extracting solution.Step (2) is the organic solvent extraction with 1～3 times of volume ratio, when the extraction mode extracts for stirring, and 4～10 ℃ of stand at low temperature layerings of room temperature.Concentrating under reduced pressure in the step (3) is that vacuum decompression concentrates, and vacuum tightness is 0.01～0.1Mpa, 40～80 ℃ of temperature, and proportion is 1.05～1.15 during 20 ℃ of concentrated solutions; The employed column chromatography filler of column chromatography for separation is wide aperture resin, polymeric amide or dextrane gel.
In order to improve the content of the cinnamophenone in the extracting solution, do not destroy the chemical structure of cinnamophenone simultaneously, extract a kind of in the preferred following solvents of solvent: the mixture of A. methyl alcohol and water, the content of methyl alcohol accounts for 50-70wt% in the mixture; B. the mixture of ethanol and water, alcoholic acid content accounts for 50-70wt% in the mixture; C. the mixture of acetone and water, the content of acetone accounts for 50-70wt% in the mixture;
Embodiment 1
Take by weighing the bright moon grass meal 1Kg of drying and crushing, added mass ratio respectively 1: 4, the water refluxing extraction of 1: 3 and 1: 33 times, for the first time kept reflux state 2 hours, second, be respectively for the third time 1.5 hours, filter, merging filtrate is evaporated to proportion 1.15 (20 ℃), stir extraction 3 times with primary isoamyl alcohol in 1: 1 ratio, merge concentrated extract, the gained enriched material is with 500g macropore XAD-7 resin absorption, ethanol water gradient elution, wherein water accounts for the ratio of ethanol water by 100wt%, interval 20wt%, gradient is decremented to 0wt%, checks effluent liquid with thin-layer chromatography Lian survey method, collection contains the effluent liquid of bright moon grass cinnamophenone, concentrating under reduced pressure gets bright moon grass cinnamophenone enriched material, again through methanol crystallization, gets the pure product of bright moon grass cinnamophenone of 1.17 gram purity 90.13%.
Embodiment 2
Take by weighing the bright moon grass meal 1Kg of drying and crushing, got 6 hours in 50 ℃ of warm lixiviates with 5 times of amount 40% ethanol, filter, decompression filtrate recycling ethanol is concentrated into proportion 1.10 (20 ℃), stirs extraction 3 times with ethyl acetate in 1: 1 ratio, combining extraction liquid, the reclaim under reduced pressure ethyl acetate, the gained enriched material is with the absorption of 500g polymeric amide, ethanol water gradient elution, wherein water accounts for the ratio of ethanol water by 100wt%, interval 10wt%, gradient is decremented to 0wt%, checks effluent liquid with the thin-layer chromatography detection method, collection contains the effluent liquid of liquorice chalcone, concentrating under reduced pressure gets bright moon grass cinnamophenone enriched material, again through the chloroform crystallization, gets the pure product of bright moon grass cinnamophenone of 2.12 gram purity 90.17%.
Embodiment 3
Take by weighing the bright moon grass meal 1Kg of drying and crushing, got 3 hours in 50 ℃ of warm lixiviates with 20 times of amount 50% acetone, extracting solution is evaporated to proportion 1.08 (20 ℃) for 60 ℃, stir extraction 2 times with propyl carbinol in 1: 3 ratio, merge concentrated extract, the gained enriched material is with 5009 macropore DlOI resin absorption, ethanol water gradient elution, wherein water account for ethanol water ratio by 100wt%, 10wt% at interval, gradient is decremented to 0wt%, check effluent liquid with the thin-layer chromatography detection method, collect the effluent liquid that contains bright moon grass cinnamophenone, concentrating under reduced pressure gets bright moon grass cinnamophenone enriched material, through the chloroform crystallization, get the pure product of bright moon grass cinnamophenone of 2.96 gram purity 90.76% again.
Embodiment 4
Take by weighing the bright moon grass meal 1Kg of drying and crushing, pressed mass ratio 1: 8 with 40% acetone, 1: 6 and 1: 6 refluxing extraction 3 times, each 2 hours, filter merging filtrate, reclaim under reduced pressure acetone, be concentrated into proportion 1.10 (20 ℃), stir extraction 3 times, combining extraction liquid, reclaim under reduced pressure ethyl acetate with ethyl acetate in 1: 1 ratio, the gained enriched material is with 500g macropore XAD-7 resin absorption, ethanol water gradient elution, wherein water account for ethanol water ratio by 100wt%, 15wt% at interval, gradient is decremented to 0wt%, check effluent liquid with the thin-layer chromatography detection method, collect the effluent liquid that contains bright moon grass cinnamophenone, concentrating under reduced pressure gets bright moon grass cinnamophenone enriched material, through methyl alcohol one chloroform crystallization, get the pure product of bright moon grass cinnamophenone of 2.21 gram purity 90.84% again.
Embodiment 5
Take by weighing the bright moon grass meal 1Kg of drying and crushing, pressed mass ratio 1: 5 with anhydrous propanone, refluxed in 1: 4 and 1: 4, kept reflux state 2 hours, filter, extract merging filtrate 3 times, reclaim under reduced pressure acetone, add water to proportion 1.15 (20 ℃) after concentrating near doing, stir extraction 3 times in 1: 1 ratio, merge concentrated extract with primary isoamyl alcohol, the gained enriched material adsorbs with the 500g polyamide resin, ethanol water gradient elution, wherein water account for ethanol water ratio by 100wt%, 20wt% at interval, gradient is decremented to 0wt%, check effluent liquid with the thin-layer chromatography detection method, collect the effluent liquid that contains bright moon grass cinnamophenone, concentrating under reduced pressure gets bright moon grass cinnamophenone enriched material, through isopropyl ether one acetone crystallization, get the pure product of bright moon grass cinnamophenone of 2.58 gram purity 91.52% again.
Embodiment 6
Take by weighing the bright moon grass meal 1Kg of drying and crushing, use 10 times respectively, 8 times, 80% acetone water refluxing extraction of 5 times of amounts 3 times, extract for the first time 3h, extract for the second time 1h, extracting 1h for the third time filters, united extraction liquid, 40 ℃ of reclaim under reduced pressure acetone are concentrated into proportion 1.05 (20 ℃), extract in 1: 3 ratio Continuous Flow with ethyl acetate, concentrated extract, the gained enriched material is with 500g macropore D10I resin absorption, ethanol water gradient elution, wherein water accounts for the ratio of ethanol water by 100wt%, interval 20wt%, gradient is decremented to 0wt%, checks effluent liquid with the thin-layer chromatography detection method, collection contains the effluent liquid of bright moon grass cinnamophenone, concentrating under reduced pressure gets bright moon grass cinnamophenone enriched material, again through isopropyl ether one acetone crystallization, gets the pure product of bright moon grass cinnamophenone of 2.73 gram purity 91.77%.
Embodiment 7
Take by weighing the bright moon grass meal 1Kg of drying and crushing, pressed mass ratio 1: 3 and 1: 2 refluxing extraction 2 times with dehydrated alcohol, each 1 hour, filter, merging filtrate, decompression recycling ethanol adds water to proportion 1.10 (20 ℃) after concentrated near the doing, and stirs extraction 3 times with ethyl acetate in 1: 1 ratio, combining extraction liquid, the reclaim under reduced pressure ethyl acetate, the gained enriched material is with the absorption of 500g polymeric amide, ethanol water gradient elution, wherein water accounts for the ratio of ethanol water by 100wt%, interval 15wt%, gradient is decremented to 0wt%, checks effluent liquid with the thin-layer chromatography detection method, collection contains the effluent liquid of bright moon grass cinnamophenone, concentrating under reduced pressure gets bright moon grass cinnamophenone enriched material, again through hexanol one isopropyl ether crystallization, gets the pure product of bright moon grass cinnamophenone of 2.07 gram purity 91.82%.
Embodiment 8
Take by weighing the bright moon grass meal 1Kg of drying and crushing, pressed mass ratio 1: 8 with 80% methyl alcohol, 1: 6 and 1: 4 refluxing extraction 3 times, each 2 hours, filter merging filtrate, reclaim under reduced pressure methyl alcohol, be concentrated into proportion 1.10 (20 ℃), stir extraction 3 times, combining extraction liquid, reclaim under reduced pressure propyl carbinol with propyl carbinol in 1: 1 ratio, the gained enriched material adsorbs with the 500g polymeric amide, ethanol water gradient elution, wherein water account for ethanol water ratio by 100wt%, 20wt% at interval, gradient is decremented to 0wt%, check effluent liquid with the thin-layer chromatography detection method, collect the effluent liquid that contains bright moon grass cinnamophenone, concentrating under reduced pressure gets bright moon grass cinnamophenone enriched material, through ethanol one isopropyl ether crystallization, get the pure product of bright moon grass cinnamophenone of 2.02 gram purity 92.12% again.
Embodiment 9
Take by weighing the bright moon grass meal 1Kg of drying and crushing, 80% ethanol with 20 times of amounts at room temperature soaks 2h, extract with the cold method of oozing then, diacolation speed is 10mL/min, the percolate concentrating under reduced pressure, when being concentrated into proportion and being 1.08 (20 ℃), stir extraction 3 times with water saturated propyl carbinol in 1: 1 ratio, combining extraction liquid and concentrating under reduced pressure reclaim propyl carbinol, and the gained enriched material is with 500g macropore D10I resin absorption, ethanol water gradient elution, wherein water accounts for the ratio of ethanol water by 100wt%, interval 20wt%, gradient is decremented to 0wt%, checks effluent liquid with the thin-layer chromatography detection method, collection contains the effluent liquid of cinnamophenone, concentrating under reduced pressure gets the cinnamophenone enriched material, again through isopropyl ether one acetone crystallization, gets the pure product of cinnamophenone of 2.82 gram purity 92.21%.
Embodiment 10
Take by weighing the bright moon grass meal IKg of drying and crushing, soaked 3 hours 45 ℃ of following temperature with 8 times of amount 40% methyl alcohol, filter, repeat 1 time, merging filtrate, filtrate decompression is concentrated into proportion 1.08 (20 ℃), stir extraction 3 times with chloroform in 1: 1 ratio, concentrated extract, the gained enriched material separates with 500g SephadexLH-20,60% methanol aqueous solution wash-out, check effluent liquid with the thin-layer chromatography detection method, collect the effluent liquid that contains bright moon grass cinnamophenone, concentrating under reduced pressure gets bright moon grass cinnamophenone enriched material, through isopropyl ether one acetone refining, get the pure product of bright moon grass cinnamophenone of 2.52 gram purity 92.52% again.
Embodiment 11
Take by weighing the bright moon grass meal 1Kg of drying and crushing, pressed mass ratio 1: 8 with 50% methyl alcohol, 1: 6 and 1: 6 refluxing extraction 3 times, united extraction liquid, reclaim under reduced pressure methyl alcohol, be concentrated into proportion 1.12 (20 ℃), stir extraction 3 times with primary isoamyl alcohol in 1: 1 ratio, merge concentrated extract, the gained enriched material is with 500g macropore AB-8 resin absorption, ethanol water gradient elution, wherein water accounts for the ratio of ethanol water by 100wt%, interval 15wt%, gradient is decremented to 0wt%, checks effluent liquid with the thin-layer chromatography detection method, collection contains the effluent liquid of liquorice chalcone, concentrating under reduced pressure gets bright moon grass cinnamophenone enriched material, again through isopropyl ether one acetone crystallization, gets the pure product of bright moon grass cinnamophenone of 2.64 gram purity 93.10%.
Embodiment 12
Take by weighing the bright moon grass meal IKg of drying and crushing, at room temperature carry out diacolation with 10 times of amount anhydrous methanols, diacolation speed is 5ml/min, the percolate concentrating under reduced pressure adds water to proportion 1.10 (20 ℃) after closely doing, adopt Continuous Flow extracting and separating machine extraction 2 times with normal hexane in 1: 1 ratio, combining extraction liquid and concentrating under reduced pressure, the gained enriched material is with 500g macropore AB-8 resin absorption, acetone water gradient elution, wherein water accounts for the ratio of acetone water by 100wt%, interval 10wt%, gradient is decremented to 0wt%, checks effluent liquid with the thin-layer chromatography detection method, collection contains the effluent liquid of bright moon grass cinnamophenone, concentrating under reduced pressure gets bright moon grass cinnamophenone enriched material, again through the acetone crystallization, gets the pure product of bright moon grass cinnamophenone of 1.80 gram purity 93.70%.
In the various embodiments described above, in step (2) lining, in order to make the cinnamophenone in the bright moon grass meal fully also enter into the extraction solvent fast, when the bright moon grass meal was extracted with the extraction solvent, the extraction solvent that will contain the bright moon grass meal placed in the ultrasonic emitting scope of ultrasonic generator.When ultrasonic wave is propagated,, can produce little cavity in extraction solvent inside owing to extract the high vibration of solvent particulate in the extraction solvent.These little cavities swell rapidly and are closed, can make to extract fierce effect of impact takes place between the solvent particulate, play good mixing effect, thereby add the dissolving of fast solute, quicken chemical reaction, and then make the cinnamophenone in the bright moon grass meal fully also enter into the extraction solvent fast.
From the various embodiments described above, as can be seen, when the cold solvent soaking bright moon grass meal that oozes method with 10～12 times of mass ratioes, temperature is soaked the solvent soaking bright moon grass meal of method with 8～20 times of mass ratioes, circumfluence method is during with the solvent soaking bright moon grass meal of 5～10 times of mass ratioes, bright moon grass meal etc. quality can obtain the pure product of more cinnamophenone, so extract the preferred above-mentioned parameter of amount of solvent in the step (1).
More than show and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that describes in the foregoing description and the specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (10)
1. the extracting method of high purity bright moon grass cinnamophenone is characterized in that, comprises the steps:
(1) extracts, the bright moon grass is dried and crushed into the bright moon grass meal, the bright moon grass meal is extracted with the extraction solvent, obtain extracting solution;
(2) extraction with an organic solvent extracts extracting solution, obtains organic solvent extraction phase and extracting phase;
(3) separate, organic solvent extraction is carried out concentrating under reduced pressure mutually, obtain enriched material, enriched material is passed through column chromatography for separation, the eluent wash-out, acquisition contains the effluent liquid of cinnamophenone, and this effluent liquid of concentrating under reduced pressure, gets the cinnamophenone enriched material;
(4) crystallization promptly gets the pure product of cinnamophenone with the cinnamophenone enriched material with the organic solvent crystallization.
2. the extracting method of high purity bright moon grass cinnamophenone according to claim 1 is characterized in that,
In the step (1), the bright moon grass meal is comprised with the method that the extraction solvent extracts: coldly ooze method, temperature is soaked method or circumfluence method; Described extraction solvent is a kind of in the following solvents: the mixture of A. methyl alcohol and water, and the content of methyl alcohol accounts for 0-100wt% in the mixture; B. the mixture of ethanol and water, alcoholic acid content accounts for 0-100wt% in the mixture; C. the mixture of acetone and water, the content of acetone accounts for 0-100wt% in the mixture;
In the step (2), organic solvent adopts the mode that stirs extraction or adopt Continuous Flow extracting and separating machine to extract to extract and carries extracting solution; Described organic solvent is a kind of in propyl carbinol, ethyl acetate, normal hexane, chloroform or the primary isoamyl alcohol;
In the step (3), when obtaining enriched material, can reclaim organic solvent wherein; Eluent is made up of aqueous ethanolic solution or methanol aqueous solution or aqueous acetone solution, and wherein the ratio that accounts for of water is 100-0wt%, degree of grade or gradient elution; Check effluent liquid with thin-layer chromatography detection method or high performance liquid chromatography, collect the effluent liquid that contains cinnamophenone;
In the step (4), described organic solvent is acetone, ethanol, methyl alcohol, isopropyl ether, chloroform or their mixed solvent.
3. the extracting method of high purity bright moon grass cinnamophenone according to claim 2, it is characterized in that, the extracting solution vacuum decompression to be concentrated into vacuum tightness before be 0.01～0.1Mpa carrying out step (2), 40～80 ℃ of temperature, and proportion is 1.05～1.15 during 20 ℃ of concentrated solutions; Reclaim the organic solvent in the extracting solution.
4. the extracting method of high purity bright moon grass cinnamophenone according to claim 3, it is characterized in that, the cold method of oozing in the step (1) is extracted with the method for diacolation then at room temperature with the solvent soaking bright moon grass meal of 10～15 times of mass ratioes, and extraction time is 1～5 time; Temperature in the step (1) soak method under 30～45 ℃ of temperature with solvent soaking bright moon grass meal, the stirring of 5～25 times of mass ratioes and be incubated 3～6 hours; Circumfluence method in the step (1) is the solvent soaking bright moon grass meal with 2～15 times of mass ratioes, and heating makes solvent refluxing and kept reflux state 1～5 hour.
5. the extracting method of high purity bright moon grass cinnamophenone according to claim 4, it is characterized in that, the cold solvent soaking bright moon grass meal that oozes method with 10～12 times of mass ratioes, temperature is soaked the solvent soaking bright moon grass meal of method with 8～20 times of mass ratioes, and circumfluence method is with the solvent soaking bright moon grass meal of 5～10 times of mass ratioes.
6. the extracting method of high purity bright moon grass cinnamophenone according to claim 3, it is characterized in that the concentrating under reduced pressure in the step (3) is that vacuum decompression concentrates, vacuum tightness is 0.01～0.1Mpa, proportion is 1.05～1.15 when 40～80 ℃ of temperature, 20 ℃ of concentrated solutions; The employed column chromatography filler of column chromatography for separation is wide aperture resin, polymeric amide or dextrane gel.
7. the extracting method of high purity bright moon grass cinnamophenone according to claim 3 is characterized in that step (2) is the organic solvent extraction with 1～3 times of volume ratio, when the extraction mode extracts for stirring, and 4～10 ℃ of stand at low temperature layerings of room temperature.
8. according to the extracting method of any described high purity bright moon grass cinnamophenone in the claim 2 to 7, it is characterized in that, in the step (1), when the bright moon grass meal was extracted with the extraction solvent, the extraction solvent that will contain the bright moon grass meal placed in the ultrasonic emitting scope of ultrasonic generator.
9. the extracting method of high purity bright moon according to claim 8 grass cinnamophenone is characterized in that, described extraction solvent is a kind of in the following solvents: the mixture of A. methyl alcohol and water, and the content of methyl alcohol accounts for 50-70wt% in the mixture; B. the mixture of ethanol and water, alcoholic acid content accounts for 50-70wt% in the mixture; C. the mixture of acetone and water, the content of acetone accounts for 50-70wt% in the mixture.
10. the extracting method of high purity bright moon grass cinnamophenone according to claim 9, it is characterized in that, at room temperature carry out diacolation with 10 times of amount anhydrous methanols, diacolation speed is 5ml/min, the percolate concentrating under reduced pressure adds water to proportion 1.10 (20 ℃) after closely doing, adopt Continuous Flow extracting and separating machine extraction 2 times with normal hexane in 1: 1 ratio, combining extraction liquid and concentrating under reduced pressure, the gained enriched material is with macropore AB-8 resin absorption, acetone water gradient elution, wherein water account for acetone water ratio by 100wt%, 10wt% at interval, gradient is decremented to 0wt%, check effluent liquid with the thin-layer chromatography detection method, collect the effluent liquid that contains bright moon grass cinnamophenone, concentrating under reduced pressure gets the cinnamophenone enriched material, through the acetone crystallization, get the pure product of careless cinnamophenone again.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102783524A (en) * | 2012-08-08 | 2012-11-21 | 鲜活果汁工业（昆山）有限公司 | Preparation method and purpose of chalcone flavonol derivatives of black bean extracts |
| CN105859538A (en) * | 2016-06-08 | 2016-08-17 | 青海省青海湖药业有限公司 | Purification method of licochalcone A |
| CN113321680A (en) * | 2021-04-28 | 2021-08-31 | 潘惟谦 | Production process for effectively extracting organic germanium, biological selenium and chalcone from angelica keiskei |
-
2010
- 2010-03-18 CN CN2010101274250A patent/CN102190571A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102783524A (en) * | 2012-08-08 | 2012-11-21 | 鲜活果汁工业（昆山）有限公司 | Preparation method and purpose of chalcone flavonol derivatives of black bean extracts |
| CN105859538A (en) * | 2016-06-08 | 2016-08-17 | 青海省青海湖药业有限公司 | Purification method of licochalcone A |
| CN113321680A (en) * | 2021-04-28 | 2021-08-31 | 潘惟谦 | Production process for effectively extracting organic germanium, biological selenium and chalcone from angelica keiskei |
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Application publication date: 20110921 |