CN102850374A - Method for preparing jolkinolide B - Google Patents
Method for preparing jolkinolide B Download PDFInfo
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- CN102850374A CN102850374A CN201210363016XA CN201210363016A CN102850374A CN 102850374 A CN102850374 A CN 102850374A CN 201210363016X A CN201210363016X A CN 201210363016XA CN 201210363016 A CN201210363016 A CN 201210363016A CN 102850374 A CN102850374 A CN 102850374A
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- CN
- China
- Prior art keywords
- extraction
- heptane
- beijing euphorbia
- lactone
- jolkinolide
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
Abstract
The invention belongs to the field of natural pharmaceutical chemistry and relates to a method for preparing jolkinolide B. The method comprises the following steps: taking euphorbia jolkini roots, crushing, screening by a sieve with 40-60 meshes, feeding the euphorbia jolkini roots to an extraction kettle, carrying out supercritical co2 extraction by using ethanol water solution with the volume percentage of 75% as an entrainer, collecting extract liquid, degreasing with heptane after recovering ethanol, carrying out high-speed counter-current chromatography by using heptane-ethyl acetate-acetonitrile-water as a solvent system and drying the fraction to obtain the jolkinolide B. Jolkinolide B products prepared by the method have the advantages of having no pollution and high yield, and the method is suitable for industrial preparation of jolkinolide B.
Description
Technical field
The invention belongs to the Natural Medicine Chemistry field, particularly relate to a kind of employing supercritical CO
2Extraction and high speed adverse current chromatogram isolation technique prepare the method for southern root of Beijing euphorbia lactone B.
Background technology
South root of Beijing euphorbia lactone B is diterpene-kind compound, mp.212 ℃ (decomposition), the needle shape that is white in color, molecular formula C
20H
26O
4, molecular weight 330.42.South root of Beijing euphorbia lactone B extensively exists in natural phant, mainly separates obtaining from euphorbia plant.Pharmacological research shows, southern root of Beijing euphorbia lactone B has the effect that promotes that nerve growth factor forms, and can be used for treating spinal injury, peripheral nerve damage, diabetic neuropathy and myatrophy outside hardening.In addition, also have antitumour activity, the antitumour activity test shows in the animal body, and southern root of Beijing euphorbia lactone B has the activity of the Growth of Cells such as obvious inhibition S180, ehrlich carcinoma, hepatic ascites.It suppresses the formation of vascular cell adhesion molecule-1, IC
50Be 0.2 μ g/mL, can be used as transfer inhibitor, be used for the treatment of arteriosclerosis, transplant rejection, chronic rheumatic arthritis and sarcoidosis etc.
Have not yet to see a large amount of method reports that prepare south root of Beijing euphorbia lactone B.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing southern root of Beijing euphorbia lactone B.
To achieve these goals, technical scheme of the present invention is as follows:
A kind of method for preparing southern root of Beijing euphorbia lactone B is characterized in that may further comprise the steps: get southern queen's delight and pulverized the 40-60 mesh sieve, add in the extraction kettle, take the aqueous ethanolic solution of volume percent as 75% as entrainment agent, adopt supercritical CO
2Extraction liquid is collected in extraction, uses the heptane degreasing behind the Recycled ethanol, again take heptane-ethyl acetate-acetonitrile-water as solvent systems, adopts high speed adverse current chromatogram to separate, and the flow point drying under reduced pressure is De Nan root of Beijing euphorbia lactone B.
Described supercritical CO
2Extraction conditions is: extraction temperature is 43-56 ℃, and extracting pressure is 25-34MPa, and separating still I temperature is 35-45 ℃, and pressure is 8-10MPa, and separating still II temperature is 25-38 ℃, and pressure is 4-7MPa, and the entrainment agent consumption is that the 1-2 of raw material doubly measures.
Described heptane-ethyl acetate-acetonitrile-water solvent systems ratio is (4-7): (2-5): (3-4): (1-2).
Supercritical CO among the present invention
2Extraction time is controlled at 2-4 hour, CO
2Flow control is at 15-22L/h.
The present invention when high speed adverse current chromatogram separating and extracting thing, be on the solvent mutually as stationary phase, lower is moving phase mutually, the acetic acid ethyl dissolution extract, the equipment rotating speed is controlled at 700-900 rpm, flow rate of mobile phase is 1.5-3.0ml/min.
Advantage of the present invention is: the process using supercritical CO
2Extraction separates southern root of Beijing euphorbia lactone B with high speed adverse current chromatogram, the loss of sepn process product-free, and preparation cycle is short, reagent can reuse, preparation amount is large, without generation of waste materials, has overcome that sample extremely adsorbs in traditional silica gel column separation process, technique is loaded down with trivial details, the technological deficiency of poor reproducibility.
Embodiment:
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 1:
Get southern queen's delight and pulverized 60 orders, get the 3kg raw material and add supercritical CO
2In the extraction kettle, opening device, adjust device parameter: extraction temperature is 56 ℃, and extracting pressure is 33.6MPa, and separating still I temperature is 45 ℃, and pressure is 9MPa, and separating still II temperature is 37 ℃, and pressure is 7MPa.Pass into CO
2Fluid, reach above-mentioned parameter after, with CO
2The extraction of liquid 20L/h flow velocity, and carry 75% aqueous ethanolic solution 6L secretly, dynamic extraction 4h collects extraction liquid, and Recycled ethanol adds the heptane degreasing, is extracted thing.Get heptane, ethyl acetate, acetonitrile, water, mix for 4:5:3:1 in proportion, get and pump into mutually separator column, until being fixed, fills mutually by separator column, rotating speed is 850rpm, simultaneously lower flow velocity with 6ml/min is pumped into, flow out from outlet end and after two-phase set up running balance, flow rate of mobile phase was adjusted to 2.0ml/min, injects the extract of moving phase dissolving until moving phase, the UV-detector monitoring, collect southern root of Beijing euphorbia lactone B flow point, continuous separate from, merge flow point drying under reduced pressure De Nan root of Beijing euphorbia lactone B, high performance liquid phase detects, content 94.2%.
Embodiment 2:
Get southern queen's delight and pulverized 40 orders, get the 5kg raw material and add supercritical CO
2In the extraction kettle, opening device, adjust device parameter: extraction temperature is 49 ℃, and extracting pressure is 28MPa, and separating still I temperature is 40 ℃, and pressure is 10MPa, and separating still II temperature is 32 ℃, and pressure is 7MPa.Pass into CO
2Fluid, reach above-mentioned parameter after, with CO
2The extraction of liquid 16L/h flow velocity, and carry 75% aqueous ethanolic solution 8L secretly, dynamic extraction 3h collects the extraction liquid Recycled ethanol, adds the heptane degreasing, is extracted thing.Get heptane, ethyl acetate, acetonitrile, water, mix for 7:3:4:2 in proportion, get and pump into mutually separator column, until being fixed, fills mutually by separator column, rotating speed is 700rpm, simultaneously lower flow velocity with 4ml/min is pumped into, flow out from outlet end and after two-phase set up running balance, flow rate of mobile phase was adjusted to 3.0ml/min, injects the extract of moving phase dissolving until moving phase, the UV-detector monitoring, collect southern root of Beijing euphorbia lactone B flow point, continuous separate from, merge flow point drying under reduced pressure De Nan root of Beijing euphorbia lactone B, high performance liquid phase detects, content 92.7%.
Embodiment 3:
Get southern queen's delight and pulverized 60 orders, get the 10kg raw material and add supercritical CO
2In the extraction kettle, opening device, adjust device parameter: extraction temperature is 43 ℃, and extracting pressure is 25MPa, and separating still I temperature is 35 ℃, and pressure is 8MPa, and separating still II temperature is 25 ℃, and pressure is 4MPa.Pass into CO
2Fluid, reach above-mentioned parameter after, with CO
2The extraction of liquid 15L/h flow velocity, and carry 75% aqueous ethanolic solution 10L secretly, dynamic extraction 2h collects extraction liquid, reclaims 75% aqueous ethanolic solution, adds the heptane degreasing, is extracted thing.Get heptane, ethyl acetate, acetonitrile, water, mix for 5:2:3:2 in proportion, get and pump into mutually separator column, until being fixed, fills mutually by separator column, rotating speed is 900rpm, simultaneously lower flow velocity with 5ml/min is pumped into, flow out from outlet end and after two-phase set up running balance, flow rate of mobile phase was adjusted to 1.5ml/min, injects the extract of moving phase dissolving until moving phase, the UV-detector monitoring, collect southern root of Beijing euphorbia lactone B flow point, continuous separate from, merge flow point drying under reduced pressure De Nan root of Beijing euphorbia lactone B product, high performance liquid phase detects, content 93.6%.
Claims (3)
1. method for preparing southern root of Beijing euphorbia lactone B is characterized in that may further comprise the steps: get southern queen's delight and pulverized the 40-60 mesh sieve, add in the extraction kettle, take the aqueous ethanolic solution of volume percent as 75% as entrainment agent, adopt supercritical CO
2Extraction liquid is collected in extraction, uses the heptane degreasing behind the Recycled ethanol, again take heptane-ethyl acetate-acetonitrile-water as solvent systems, adopts high speed adverse current chromatogram to separate, and the flow point drying under reduced pressure is De Nan root of Beijing euphorbia lactone B.
2. the method for the southern root of Beijing euphorbia of described preparation lactone B according to claim 1 is characterized in that described supercritical CO
2Extraction conditions is: extraction temperature is 43-56 ℃, and extracting pressure is 25-34MPa, and separating still I temperature is 35-45 ℃, and pressure is 8-10MPa, and separating still II temperature is 25-38 ℃, and pressure is 4-7MPa, and the entrainment agent consumption is that the 1-2 of raw material doubly measures.
3. the method for the southern root of Beijing euphorbia of described preparation lactone B according to claim 1 is characterized in that described heptane-ethyl acetate-acetonitrile-water solvent systems ratio is (4-7): (2-5): (3-4): (1-2).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210363016XA CN102850374A (en) | 2012-09-26 | 2012-09-26 | Method for preparing jolkinolide B |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210363016XA CN102850374A (en) | 2012-09-26 | 2012-09-26 | Method for preparing jolkinolide B |
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| CN102850374A true CN102850374A (en) | 2013-01-02 |
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| CN201210363016XA Pending CN102850374A (en) | 2012-09-26 | 2012-09-26 | Method for preparing jolkinolide B |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103819484A (en) * | 2014-01-22 | 2014-05-28 | 中国药科大学 | Synthesis method for natural jolkinolide A and B |
| CN106916162A (en) * | 2017-03-01 | 2017-07-04 | 中日友好医院 | A kind of preparation method of rock root of Beijing euphorbia lactone B bulk drugs |
| CN115721643A (en) * | 2021-09-01 | 2023-03-03 | 烟台资生元生物科技开发有限公司 | Application of jolkinolide B in preparation of medicine for treating tumors |
-
2012
- 2012-09-26 CN CN201210363016XA patent/CN102850374A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103819484A (en) * | 2014-01-22 | 2014-05-28 | 中国药科大学 | Synthesis method for natural jolkinolide A and B |
| CN103819484B (en) * | 2014-01-22 | 2017-04-19 | 中国药科大学 | Synthesis method for natural jolkinolide A and B |
| CN106916162A (en) * | 2017-03-01 | 2017-07-04 | 中日友好医院 | A kind of preparation method of rock root of Beijing euphorbia lactone B bulk drugs |
| CN115721643A (en) * | 2021-09-01 | 2023-03-03 | 烟台资生元生物科技开发有限公司 | Application of jolkinolide B in preparation of medicine for treating tumors |
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Application publication date: 20130102 |