CN101973972A - Method for extracting Fraxinellone from bark - Google Patents
Method for extracting Fraxinellone from bark Download PDFInfo
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- CN101973972A CN101973972A CN2010105108866A CN201010510886A CN101973972A CN 101973972 A CN101973972 A CN 101973972A CN 2010105108866 A CN2010105108866 A CN 2010105108866A CN 201010510886 A CN201010510886 A CN 201010510886A CN 101973972 A CN101973972 A CN 101973972A
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Abstract
The invention relates to a preparation method of Fraxinellone, comprising the following steps: smashing bark raw material; dipping by alkali liquor; after drying, carrying out supercritical CO2 extraction on the dipped bark raw material in an extraction kettle; adding alcohol liquid serving as entrainer; collecting analytical liquid; removing an oil layer; decompressing to recycle alcohol; and drying in vacuum to obtain the product. The method is safe and reliable, has high product content and is an efficient energy-saving preparation method.
Description
Technical field:
The invention belongs to the Separation of Natural Products field, especially relate to a kind of from Root-bark of Densefruit Pittany the method for Ti Qu Ash ketone.
Background technology:
Ash ketone, the white, needle-shaped crystals thing, fusing point: 116～117 ℃, be soluble in organic reagents such as ethanol, ethyl acetate, sherwood oil, be insoluble in water.
Molecular formula: C
14H
16O
3Molecular weight: 232.28
Structural formula:
Root-bark of Densefruit Pittany is the dry root skin of rutaceae shaggy-fruited dittany (Dictamnus dasycarpus Turcz), have dispel the wind, effect such as eliminating dampness, heat-clearing, detoxifcation, cure mainly damp and hot sore, scall scabies leprosy, skin pruritus, private parts illness such as swell and ache.Modern pharmacology studies show that Root-bark of Densefruit Pittany has anti-oxidant, antiviral, antibacterium, anti-inflammatory, various active such as antitumor.Studies show that in recent years, separating the Ash ketone that obtains from Root-bark of Densefruit Pittany is the main pharmacodynamics composition of Root-bark of Densefruit Pittany, has good protecting liver, lowering enzymes and suppresses the hepatic fibrosis isoreactivity, and have antibacterial, desinsection isoreactivity, now as a kind of novel liver disease medicine.
Mostly the method for existing document Ti Qu Ash ketone from Root-bark of Densefruit Pittany is to adopt alcohol extracting, supersound extraction, ethyl acetate extraction, silica gel column chromatography, RP-HPLC separation and purification.As " research of the chemical reference substance of Root-bark of Densefruit Pittany " that Du Chengfang etc. delivers, the method that the document adopts is alcohol extracting, ethyl acetate extraction, silica gel column chromatography separates, step Ti Qu Ash ketone such as re-crystallizing in ethyl acetate, and it is higher that this method draws De Ash ketone content, but complicated operation, the organic reagent consumption is big; The new purposes of existing patent 200810017515.7 “ Ash ketone is Ji Ash ketone aqua pesticide " method that adopts is the sherwood oil refluxing extraction; and methyl alcohol-sherwood oil mixed solvent adds separates out coarse crystallization; carry out purifying through column chromatography again, this method energy consumption is big, and the organic reagent consumption is big.
Summary of the invention:
The technical problem to be solved in the present invention provide a kind of energy consumption low, pollute Xiao De Ash ketone extracting method.
The present invention realizes by the following technical solutions:
A kind of from Root-bark of Densefruit Pittany the method for Ti Qu Ash ketone, it is characterized in that comprising following steps:
1) pre-treatment: with the Root-bark of Densefruit Pittany raw material pulverizing, add dipping by lye, leach raw material, drying;
2) extraction: will carry out the supercritical CO 2 extraction in the above-mentioned crushed after being dried thing adding extraction kettle, ethanol liquid is collected desorbed solution as entrainment agent;
3) separate: above-mentioned desorbed solution is left standstill, and layering discards oil reservoir, decompression recycling ethanol again, and vacuum-drying gets product.
Alkali lye can be a kind of in 10% liming, 5% sodium hydroxide solution in the described step 1), and soak time is 12～24 hours, adopts 60～70 ℃ hot blast when dry.
Described step 2) condition of supercritical extraction in: extraction temperature is 45～65 ℃, and extracting pressure is 30～50Mpa, CO
2Flow velocity be 20～40L/h, the extraction time is 2～3 hours, entrainment agent is 90%～99% aqueous ethanolic solution, consumption is 0.1～0.4 times of amount of material; Resolve and separate 30～40 ℃ of axe I temperature, pressure is 8～10Mpa; Separate 30～35 ℃ of axe II temperature, pressure is 6～8Mpa.
The present invention has following advantage: adopt the dipping by lye raw material, can remove water-soluble substanceses such as saponin(e flavones polysaccharide, be more conducive to extraction; Adopt supercritical CO
2Extraction, carbonic acid gas are to recycle and to environmentally safe, and supercritical state is extracted, less energy consumption, and extracting cycle is short.
Further specify 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:
Getting Root-bark of Densefruit Pittany crushed material 1Kg, add 10% liming and soaked 16 hours, leach raw material, feeds 65 ℃ of hot blasts to the crushed material thorough drying, add in the supercritical extraction jar, is 55 ℃ extracting temperature, and pressure is to extract feeding CO 2 hours under the condition of 45Mpa
2Flow velocity is 20L/h, after the to be extracted jar of homeostasis, adds the 200ml95% ethanolic soln as entrainment agent, regulating I level separation axe temperature is 30 ℃, and pressure is 10Mpa, and it is 22 ℃ that the II level is separated the axe temperature, pressure is 6Mpa, collect extraction liquid, leave standstill layering, remove oil reservoir, decompression recycling ethanol, vacuum-drying get product 1.58g, content 98.7%.
Embodiment 2:
Getting Root-bark of Densefruit Pittany crushed material 1Kg, add 5% sodium hydroxide solution and soaked 12 hours, leach raw material, feeds 60 ℃ of hot blasts to the crushed material thorough drying, add in the supercritical extraction jar, is 60 ℃ extracting temperature, and pressure is to extract feeding CO 2.5 hours under the condition of 40Mpa
2Flow velocity is 22L/h, after the to be extracted jar of homeostasis, adds the 180ml98% ethanolic soln as entrainment agent, regulating I level separation axe temperature is 25 ℃, and pressure is 8Mpa, and it is 20 ℃ that the II level is separated the axe temperature, pressure is 6Mpa, collect extraction liquid, leave standstill layering, remove oil reservoir, decompression recycling ethanol, vacuum-drying get product 1.43g, content 97.9%.
Embodiment 3:
Getting Root-bark of Densefruit Pittany crushed material 5Kg, add 5% sodium hydroxide solution and soaked 20 hours, leach raw material, feeds 65 ℃ of hot blasts to the crushed material thorough drying, add in the supercritical extraction jar, is 50 ℃ extracting temperature, and pressure is to extract feeding CO 3 hours under the condition of 60Mpa
2Flow velocity is 35L/h, after the to be extracted jar of homeostasis, adds the 1L85% ethanolic soln as entrainment agent, regulating I level separation axe temperature is 22 ℃, and pressure is 9Mpa, and it is 18 ℃ that the II level is separated the axe temperature, pressure is 7Mpa, collect extraction liquid, leave standstill layering, remove oil reservoir, decompression recycling ethanol, vacuum-drying get product 7.2g, content 98.1%.
Embodiment 4:
Getting Root-bark of Densefruit Pittany crushed material 5Kg, add 10% liming and soaked 18 hours, leach raw material, feeds 65 ℃ of hot blasts to the crushed material thorough drying, add in the supercritical extraction jar, is 48 ℃ extracting temperature, and pressure is to extract feeding CO 2.5 hours under the condition of 50Mpa
2Flow velocity is 40L/h, after the to be extracted jar of homeostasis, adds the 1.2L95% ethanolic soln as entrainment agent, regulating I level separation axe temperature is 24 ℃, and pressure is 11Mpa, and it is 20 ℃ that the II level is separated the axe temperature, pressure is 7Mpa, collect extraction liquid, leave standstill layering, remove oil reservoir, decompression recycling ethanol, vacuum-drying get product 8.3g, content 97.3%.
Claims (3)
1. from Root-bark of Densefruit Pittany, put forward the method for getting Ash ketone for one kind, it is characterized in that comprising following steps:
1) pre-treatment: with the Root-bark of Densefruit Pittany raw material pulverizing, add dipping by lye, leach raw material, drying;
2) extraction: will carry out the supercritical CO 2 extraction in the above-mentioned crushed after being dried thing adding extraction kettle, ethanol liquid is collected desorbed solution as entrainment agent;
3) separate: above-mentioned desorbed solution is left standstill, and layering discards oil reservoir, decompression recycling ethanol again, and vacuum-drying gets product.
2. as claimed in claim 1 from Root-bark of Densefruit Pittany the method for Ti Qu Ash ketone, it is characterized in that alkali lye in the described step 1) can be a kind of in 10% liming, 5% sodium hydroxide solution, soak time is 12～24 hours, adopts 60～70 ℃ hot blast when dry.
3. as claimed in claim 1 from Root-bark of Densefruit Pittany the method for Ti Qu Ash ketone, it is characterized in that described step 2) in the condition of supercritical extraction: extraction temperature is 45～65 ℃, and extracting pressure is 30～50Mpa, CO
2Flow velocity be 20～40L/h, the extraction time is 2～3 hours, entrainment agent is 90%～99% aqueous ethanolic solution, consumption is 0.1～0.4 times of amount of material; Resolve and separate 30～40 ℃ of axe I temperature, pressure is 8～10Mpa; Separate 30～35 ℃ of axe II temperature, pressure is 6～8Mpa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105108866A CN101973972A (en) | 2010-10-19 | 2010-10-19 | Method for extracting Fraxinellone from bark |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105108866A CN101973972A (en) | 2010-10-19 | 2010-10-19 | Method for extracting Fraxinellone from bark |
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| CN101973972A true CN101973972A (en) | 2011-02-16 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2010105108866A Pending CN101973972A (en) | 2010-10-19 | 2010-10-19 | Method for extracting Fraxinellone from bark |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102648941A (en) * | 2011-02-28 | 2012-08-29 | 中国医学科学院药用植物研究所 | New application for antioxidation action of cortex dictamni extract |
-
2010
- 2010-10-19 CN CN2010105108866A patent/CN101973972A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102648941A (en) * | 2011-02-28 | 2012-08-29 | 中国医学科学院药用植物研究所 | New application for antioxidation action of cortex dictamni extract |
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Application publication date: 20110216 |