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Preparation method of lathyrol

A technology of diterpene alcohol and caperia sativa, which is applied in the field of separation and purification of traditional Chinese medicine, can solve the problems of inability to apply large-scale industrial production and the difficulty of compound separation, and achieve the effects of shortening hydrolysis time, reducing production cost, and less solvent consumption

Active Publication Date: 2018-03-09
R & D CENT OF TIANJIN ZHONGXIN PHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method is to separate the compound first, and then carry out hydrolysis. On the one hand, this operation is difficult to fully enrich the compound with the capitol diterpene alcohol as the mother nucleus. On the other hand, the separation of the compound also has certain difficulties. Therefore, Cannot be applied to industrial mass production

Method used

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  • Preparation method of lathyrol
  • Preparation method of lathyrol
  • Preparation method of lathyrol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] a, medicinal material pulverization: choose 10kg of 10kg of daughter fruit, pulverize into granules;

[0033] b. Reflux extraction and concentration: reflux extract the crushed Stephania chinensis medicinal material once with 95% ethanol for 2 hours each time, and add 60L 95% ethanol for each extraction. After the extraction is completed, the extract is pumped into the concentration tank and concentrated to a thick paste;

[0034] c. Alkaline hydrolysis: add 50L 0.1mol / LNaOH / 95% alcohol solution to the above thick paste and hydrolyze for 12 hours;

[0035] d. Neutralization: Add about 6L of 1% hydrochloric acid to the above-mentioned alkaline hydrolyzate to adjust the pH value to 7;

[0036] e. Silica gel column chromatography: Concentrate the above-mentioned neutralized hydrolyzate to a thick extract (about 200g) under reduced pressure, then mix the sample with 200g of silica gel, dry it, and add it to the chromatographic column with 1.0Kg of silica gel in the lower l...

Embodiment 2

[0039] a, medicinal material pulverization: choose 10kg of 10kg of daughter fruit, pulverize into granules;

[0040] b. Reflux extraction and concentration: reflux extract the crushed Stephania chinensis medicinal material with 95% ethanol for 3 times, each time for 4 hours, and add 150L of 95% ethanol for each extraction. After the extraction is completed, the three extractions are combined, pumped into the concentration tank and concentrated to a thick paste;

[0041] c. Alkaline hydrolysis: add 100L 0.1mol / LNaOMe / 95% alcohol solution to the above-mentioned thick paste to hydrolyze for 24 hours;

[0042] d. Neutralization: Add about 0.8L of 15% hydrochloric acid to the above-mentioned alkaline hydrolyzate to adjust the pH value to 7;

[0043] e. Silica gel column chromatography: Concentrate the above-mentioned neutralized hydrolyzate to a thick extract (about 240g) under reduced pressure, then mix the sample with 250g of silica gel, dry it, and add it to the chromatography ...

Embodiment 3

[0046] a, medicinal material pulverization: choose 10kg of 10kg of daughter fruit, pulverize into granules;

[0047] b. Reflux extraction and concentration: reflux extraction of the crushed Stephania chinensis with methanol for 2 hours each time, adding 60L of methanol for each extraction. After the extraction is completed, the extract is pumped into the concentration tank and concentrated to a thick paste;

[0048] c. Alkaline hydrolysis: add 50L 0.25mol / LNaOH / 95% alcohol solution to the above thick paste and hydrolyze for 2 hours;

[0049] d. Neutralization: add about 5.0L 3% hydrochloric acid to the above-mentioned alkaline hydrolyzate to adjust the pH value to 7;

[0050]e. Silica gel column chromatography: Concentrate the above-mentioned neutralized hydrolyzate to a thick extract (about 210g) under reduced pressure, then mix the sample with 250g of silica gel, dry it, and add it to the chromatography column with 1.0Kg of silica gel in the lower layer to carry out Chroma...

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Abstract

The invention discloses a preparation method of lathyrol. The preparation method includes: a, taking semen euphorbia lathyris (which is bought in the market) as a raw material, and pulverizing semen euphorbia lathyris to obtain semen euphorbia lathyris powder; b, performing reflux extraction with a proper solvent, combining extracts, and performing reduced-pressure concentration to obtain stiff paste; c, adding alkali liquor to the stiff paste for hydrolysis; d, adding acid to the alkali-hydrolyzed liquid to adjust the pH value to 6-7; e, performing reduced-pressure concentration to the neutralized hydrolysate till stiff paste is obtained, and performing silica gel column chromatography to obtain coarse lathyrol; and f, re-crystallizing the obtained coarse lathyrol with a mixed solvent ofpetroleum ether and ethyl acetate to obtain a crystal product. The preparation method is simple to operate, less in solvent consumption, and stable in process, and is suitable for laboratorial and industrial preparation.

Description

technical field [0001] The invention relates to a method for preparing diterpene alcohol of Caperia spp. and belongs to the technical field of separation and purification of traditional Chinese medicines. Background technique [0002] Caperia diterpene alcohol, also known as stephenia diterpene alcohol, English name lathyrol, molecular formula C 20 h 30 o 4 , with a molecular weight of 334, is derived from Euphorbiaceae Euphorbi genus Euphorbia, and its derivatives show better cytotoxicity and tumor cell inhibition. Its structural formula is as follows: [0003] [0004] Qianjinzi is the dry and mature seed of Euphorbia lahyris L., a plant of the Euphorbia family. It is pungent in taste, warm in nature, and poisonous. Pain, constipation, amenorrhea due to blood stasis, external treatment of persistent warts and warts. Dianjinzi mainly contains a large amount of fatty oil, and also contains compounds such as diterpenes, coumarins, and volatile oils. Modern research sh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/737C07C45/64C07C45/78C07C45/79C07C45/81
CPCC07C45/64C07C45/78C07C45/79C07C45/81C07C49/737
Inventor 吴晓磊孙传腾潘勤管玉真田福莹傅小萌
Owner R & D CENT OF TIANJIN ZHONGXIN PHARM
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