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Preparation method of active pharmaceutical ingredient jolkinolide B

A technology of spurge lactone and raw material medicine, applied in the field of natural organic chemistry, can solve the problems of high production cost, complicated operation, low product yield and the like, achieve high yield, improve yield, simple and practical technological process Effect

Active Publication Date: 2017-07-04
CHINA JAPAN FRIENDSHIP HOSPITAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be seen that some of these existing technologies disclose a rough separation process for extracting euphoride B together with other active ingredients, and the targeting of the extraction of euphoride B with the best effect is not strong; Or use large-scale equipment, complex operation, high production cost and low product yield, which is not suitable for industrialized large-scale production

Method used

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  • Preparation method of active pharmaceutical ingredient jolkinolide B
  • Preparation method of active pharmaceutical ingredient jolkinolide B
  • Preparation method of active pharmaceutical ingredient jolkinolide B

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) Grind 500g dried root of Euphorbia chamaejasme into coarse powder, add 6L 60% ethanol for reflux extraction for 3h, filter, add 5L 60% ethanol to the filter residue for reflux extraction for 2h, filter, add 5L 60% ethanol for filter residue Reflux for extraction for 1 hour, filter, combine the extracts, concentrate under reduced pressure until there is no alcohol smell, and the density is 1.11 to obtain a concentrated solution (about 76 g);

[0043] (2) After the concentrated solution was dispersed with a small amount of water, it was extracted 4 times with 2 times the volume of ethyl acetate, the ethyl acetate phase was combined, and the ethyl acetate was recovered to obtain extract I (about 6.5 g);

[0044] (3) After dissolving the extract I with 20% ethanol, put it on the AB-8 macroporous adsorption resin column, pack the column by wet method (the ratio of sample volume to column resin volume is 1:3), and first elute with 20% ethanol 5BV, discarded; 8BV was elute...

Embodiment 2

[0047] (1) Grind 500g dried root of Euphorbia chamaejasme into coarse powder, add 6L 80% ethanol for reflux extraction for 3h, filter, add 5L80% ethanol to the filter residue for reflux extraction for 2h, filter, add 5L 80% ethanol for reflux extraction After 1 hour, filter, combine the extracts, concentrate under reduced pressure until there is no alcohol smell, and the density is 1.12 to obtain a concentrated solution (about 80 g).

[0048] (2) After the concentrated solution was dispersed with a small amount of water, it was extracted 4 times with 2.5 times the volume of ethyl acetate, the ethyl acetate phase was combined, and the ethyl acetate was recovered to obtain extract I (about 5.5 g);

[0049] (3) After dissolving the extract I with 30% ethanol, put it on the D101 macroporous adsorption resin column, and wet-pack the column (the ratio of the sample volume to the column resin volume is 1: 3), and first elute 5BV with 30% ethanol, Discard; then elute 8BV with 85% etha...

Embodiment 3

[0052] (1) Grind 500g dried root of Euphorbia chamaejasme into coarse powder, add 6L 95% ethanol for reflux extraction for 3h, filter, add 5L 95% ethanol to the filter residue for reflux extraction for 2h, filter, add 5L 95% ethanol for filter residue Reflux for extraction for 1 hour, filter, combine the extracts, concentrate under reduced pressure until there is no alcohol smell, and the density is 1.12 to obtain a concentrated solution (about 85 g).

[0053] (2) After the concentrated solution was dispersed with a small amount of water, it was extracted 4 times with 3 times the volume of ethyl acetate, the ethyl acetate phase was combined, and the ethyl acetate was recovered to obtain extract I (about 7.0 g);

[0054] (3) After dissolving the extract I with 40% ethanol, put it on the ADS-17 macroporous adsorption resin column, pack the column by wet method (the ratio of sample volume to column resin volume is 1:3), and first elute with 40% ethanol 5BV, discarded; then 8BV wa...

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Abstract

The invention belongs to the field of natural organic chemistry and relates to a preparation method of jolkinolide B. In the invention, dry roots of a plant, Euphorbia fischeriana Steud, belongs to Euphorbia in Euphorbiaceae are employed as a raw material, which is subjected to the processes including crushing, solvent extraction, organic solvent extraction, macroporous adsorption resin column chromatography, polyamide resin column chromatography, organic solvent extraction, drying and the like so as to produce the jolkinolide B. The method, compared with conventional methods for enriching the jolkinolide B, has simple processes and low cost, is increased in product yield on the basis of medicine, and has good industrial adaptability.

Description

technical field [0001] The invention belongs to the field of natural organic chemistry, and in particular relates to a method for enriching eupholactone B from Euphorbia chamaejasbae. [0002] technical background [0003] Jolkinolide B (jolkinolide B) is an abietane-type diterpenoid compound contained in the root of Euphorbia fischeriana Steud., and its structural formula is as follows: [0004] [0005] 【CAS】37905-08-1 [0006] 【Molecular formula and molecular weight】C 20 h 26 o 4 ;330 [0007] 【Chemical Class】Diterpene [0008] 【Physical and chemical properties】Like white powder, easily soluble in dichloromethane, chloroform, ethyl acetate, acetone, etc. mp 212°C. UV lambda max (EtOH): 242nm (ε16580). IR υ max (KBr)cm -1 : 1785, 2950, ​​2865, 1190, 1210. MS m / z: 330 (M + ). [0009] Jolkinolide B (Jolkinolide B) is an abietane-type diterpene, which widely exists in Euphorbiaceae plants. As the main active ingredient of Euphorbia chamaejasma, Jolkinolide B ...

Claims

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Application Information

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IPC IPC(8): C07D493/20
CPCC07D493/20
Inventor 张维库续洁琨赫军张佳
Owner CHINA JAPAN FRIENDSHIP HOSPITAL
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