CN102863414A - Method for extracting fraxinellone through subcritical fluid - Google Patents
Method for extracting fraxinellone through subcritical fluid Download PDFInfo
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- CN102863414A CN102863414A CN 201210353594 CN201210353594A CN102863414A CN 102863414 A CN102863414 A CN 102863414A CN 201210353594 CN201210353594 CN 201210353594 CN 201210353594 A CN201210353594 A CN 201210353594A CN 102863414 A CN102863414 A CN 102863414A
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- fraxinellone
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- macroporous resin
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Abstract
The invention discloses a method for extracting fraxinellone through subcritical fluid. The method comprises the steps as follows: drying and crushing cortex dictamni, and adding to a subcritical extracting kettle; adding a polar organic solvent, and dynamically extracting for 30 to 80 minutes at 80 to 120 DEG C under pressure of 0.2 to 1Mpa to obtain extract; recovering reagent under reduced pressure to obtain concentrated solution; adding the concentrated solution to macroporous resin to be absorbed; eluting with 4 to 7 times of 60-90% ethanol solution based on column volume; concentrating eluant; extracting the concentrated eluant with petroleum ether for two to three times; collecting the petroleum ether layer, and recovering the reagent to obtain fraxinellone. With the adoption of the method for extracting fraxinellone disclosed by the invention, little solvent is used, energy comsumption is low, high efficiency is ensured, and industrial operation is easy to carry out.
Description
Technical field
The invention belongs to biological technical field, particularly relate to a kind of method of utilizing subcritical fluid extraction to get fraxinellone.
Background technology
Root-bark of Densefruit Pittany be the rutaceae shaggy-fruited dittany (
Dictamnus dasycarpus Turcz) the dry root skin, have dispel the wind, the effect such as eliminating dampness, heat-clearing, detoxifcation, cure mainly damp and hot sore, scall scabies leprosy, skin pruritus, the private parts illness such as swell and ache.Studies show that in recent years, fraxinellone are the main pharmacodynamics composition of Root-bark of Densefruit Pittany, have good protecting liver, lowering enzymes and suppress the hepatic fibrosis isoreactivity, and have antibacterial, desinsection isoreactivity, now as a kind of novel hepatosis treating medicine.
Fraxinellone is the white, needle-shaped crystals thing, and 116 ~ 117 ℃ of fusing points are soluble in the organic reagents such as ethanol, ethyl acetate, sherwood oil, are insoluble in water.Molecular formula: C
14H
16O
3, molecular weight: 232.28,
Structural formula:
The preparation method of fraxinellone adopts conventional organic reagent to extract and supercritical CO
2Patent (the new purposes of 200810017515.7) “ fraxinellones is Ji the fraxinellone 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, the method energy consumption is large, and the organic reagent consumption is large.(application number: 201010510886.6) method of Ti Qu fraxinellone " a kind of from Root-bark of Densefruit Pittany ", this patent adopts SCF-CO 2, is a kind of efficient, Clean method, is difficult to industrialization but equipment manufacturing cost is high for another example.
Subcritical abstraction is to utilize subcritical fluids as extraction agent, in the pressurized vessel of airtight, anaerobic, low pressure, according to the similar principle that mixes of organism, by extraction material and the molecular diffusion process of extraction agent in immersion process, the composition that reaches in the solid materials is transferred in the liquid extraction agent fully, the process of passing through reduction vaporization again finally obtains a kind of novel extraction and the isolation technique of purpose product with extraction agent and purpose product separation.Subcritical fluid extraction is compared other separation method and is compared advantages such as having nontoxic, harmless, environmental protection, and the biologically active prod that can keep extract does not destroy, not oxidation, but and the large large-scale industrialization production of production capacity, energy-conservation, running cost is low.
Summary of the invention
The present invention seeks to the shortcomings and deficiencies of the prior art that will solve, a kind of method of utilizing subcritical fluid extraction to get fraxinellone is provided.
The present invention realizes by the following technical solutions:
A kind of method of utilizing subcritical fluid extraction to get fraxinellone is characterized in that following steps:
Extraction: the Root-bark of Densefruit Pittany crushed after being dried adds in the subcritical abstraction still, passes into the polarity organic reagent, is that 80 ~ 120 ℃, pressure are 0.2 ~ 1Mpa in temperature, dynamic extraction 30 ~ 80min, and gained extraction liquid reclaim under reduced pressure reagent gets concentrated solution;
Purifying: above-mentioned concentrated solution adds in the macroporous resin and adsorbs, and with 4 ~ 7 times of column volume 60-90% ethanolic soln wash-outs, elutriant is concentrated, and concentrated solution petroleum ether extraction 2 ~ 3 times are collected petroleum ether layer and reclaimed reagent ， De fraxinellone.
Described polarity organic reagent is the aqueous solution of methyl alcohol, ethanol or acetone.
The optional non-polar macroporous resin of described macroporous resin or low-pole macroporous resin.
Advantage of the present invention is: adopt subcritical abstraction to separate with macroporous resin column, extraction efficiency is high, and solvent load is few, and purification step is simple, and whole technique is easy to the industrialization operation.
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:
The Root-bark of Densefruit Pittany drying and crushing is got 1Kg, adds in the subcritical abstraction still, passing into the 5L80% ethanolic soln, is 110 ℃ in temperature, and pressure is under the 0.4 Mpa state, dynamic extraction 40min, extraction liquid reclaim under reduced pressure reagent, concentrated solution adds in the D101 macroporous resin and adsorbs, with 5 times of column volumes, 70% ethanolic soln wash-out, elutriant is concentrated, concentrated solution petroleum ether extraction 3 times are collected petroleum ether layer and are reclaimed reagent, De Baise fraxinellone powder 1.4g.
Embodiment 2:
The Root-bark of Densefruit Pittany drying and crushing is got 1Kg, adds in the subcritical abstraction still, passing into the 6L70% methanol solution, is 120 ℃ in temperature, and pressure is under the 0.8 Mpa state, dynamic extraction 50min, extraction liquid reclaim under reduced pressure reagent, concentrated solution adds in the AB-8 macroporous resin and adsorbs, with 4 times of column volumes, 80% ethanolic soln wash-out, elutriant is concentrated, concentrated solution petroleum ether extraction 2 times are collected petroleum ether layer and are reclaimed reagent, De Baise fraxinellone powder 1.7g.
Embodiment 3:
The Root-bark of Densefruit Pittany drying and crushing is got 1Kg, adds in the subcritical abstraction still, passing into the 5L70% acetone soln, is 90 ℃ in temperature, and pressure is under the 0.5 Mpa state, dynamic extraction 60min, extraction liquid reclaim under reduced pressure reagent, concentrated solution adds in the HZ-816 macroporous resin and adsorbs, with 4 times of column volumes, 90% ethanolic soln wash-out, elutriant is concentrated, concentrated solution petroleum ether extraction 3 times are collected petroleum ether layer and are reclaimed reagent, De Baise fraxinellone powder 1.6g.
Claims (3)
1. one kind is utilized subcritical fluid to extract the method for getting fraxinellone, it is characterized in that following steps:
Extraction: the Root-bark of Densefruit Pittany crushed after being dried adds in the subcritical abstraction still, passes into the polarity organic reagent, is that 80 ~ 120 ℃, pressure are 0.2 ~ 1Mpa in temperature, dynamic extraction 30 ~ 80min, and gained extraction liquid reclaim under reduced pressure reagent gets concentrated solution;
Purifying: above-mentioned concentrated solution adds in the macroporous resin and adsorbs, and with 4 ~ 7 times of column volumes, 60 ~ 90% ethanolic soln wash-outs, elutriant is concentrated, and concentrated solution petroleum ether extraction 2-3 time collected petroleum ether layer and reclaimed reagent ， De fraxinellone.
2. a kind of method of utilizing subcritical fluid extraction to get fraxinellone as claimed in claim 1 is characterized in that described polarity organic reagent is the aqueous solution of methyl alcohol, ethanol or acetone.
3. a kind of method of utilizing subcritical fluid extraction to get fraxinellone as claimed in claim 1 is characterized in that the optional non-polar macroporous resin of described macroporous resin or low-pole macroporous resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210353594 CN102863414A (en) | 2012-09-21 | 2012-09-21 | Method for extracting fraxinellone through subcritical fluid |
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| CN 201210353594 CN102863414A (en) | 2012-09-21 | 2012-09-21 | Method for extracting fraxinellone through subcritical fluid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112461977A (en) * | 2020-12-14 | 2021-03-09 | 中国科学院兰州化学物理研究所 | Phthalide compound standard substance and preparation method thereof |
| CN115414421A (en) * | 2022-08-31 | 2022-12-02 | 上海川跃生物科技有限公司 | Extraction method and application of cortex dictamni active ingredients |
-
2012
- 2012-09-21 CN CN 201210353594 patent/CN102863414A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112461977A (en) * | 2020-12-14 | 2021-03-09 | 中国科学院兰州化学物理研究所 | Phthalide compound standard substance and preparation method thereof |
| CN115414421A (en) * | 2022-08-31 | 2022-12-02 | 上海川跃生物科技有限公司 | Extraction method and application of cortex dictamni active ingredients |
| CN115414421B (en) * | 2022-08-31 | 2023-07-18 | 上海川跃生物科技有限公司 | Extraction method and application of active ingredients of cortex dictamni |
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Application publication date: 20130109 |