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Preparation method of phorbol ester compound Euphorbia Factor L2

The technology of ester compound and Euphorbia factor is applied in the field of preparation of diterpene alcohol ester compound Euphorbia factor L2, can solve the problems of low product yield, long production cycle and the like, achieves high separation efficiency, short production cycle, The effect of high operability

Inactive Publication Date: 2015-03-25
TIANJIN YAOYU BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the purification of Euphorbia FactorL2 mainly adopts conventional column chromatography, that is, the method of combining silica gel column chromatography and crystallization, which has a long production cycle and low product yield, and there is no relevant literature on the separation and purification of Euphorbia FactorL2 monomer by preparative chromatography to report

Method used

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  • Preparation method of phorbol ester compound Euphorbia Factor L2
  • Preparation method of phorbol ester compound Euphorbia Factor L2
  • Preparation method of phorbol ester compound Euphorbia Factor L2

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1. Obtaining the primary extract of QJZ

[0030] 1. Crushing:

[0031] Take Qianjinzi as a raw material, put it into a pulverizer for pulverization.

[0032] 2. Organic reagent extraction:

[0033] The stephenia powder was extracted with organic reagents, three consecutive extractions, each extraction time was 6h (heated to 60 degrees, and then heated for 6h). specific:

[0034] The first organic reagent extraction: add 2.5 kg of Stephania chinensis powder to 20 L of organic reagent, the organic reagent is ethyl acetate, stir well until the material liquid is uniform and there are no obvious lumps, turn on the water bath, extract for 6 hours, after the extraction is completed, collect the The supernatant was filtered with filter paper, and the supernatant was concentrated in a rotary evaporator and then transferred to a constant temperature blast drying oven at 60°C for drying to obtain the initial QJZ extract, which was precipitated for use;

[0035] The second org...

Embodiment 2

[0042] 1. Obtaining the primary extract of QJZ

[0043] 1. Crushing:

[0044] Take Qianjinzi as a raw material, put it into a pulverizer for pulverization.

[0045] 2. Organic reagent extraction:

[0046] The stephenia powder was extracted with organic reagents, three consecutive extractions, each extraction time was 6h (heated to 60 degrees, and then heated for 6h). specific:

[0047] The first organic reagent extraction: add 2.5 kg of Stephania chinensis powder to 20 L of organic reagent, the organic reagent is ethyl acetate, stir well until the material liquid is uniform and there are no obvious lumps, turn on the water bath, extract for 6 hours, after the extraction is completed, collect the The supernatant was filtered with filter paper, and the supernatant was concentrated in a rotary evaporator and then transferred to a constant temperature blast drying oven at 60°C for drying to obtain the initial QJZ extract, which was precipitated for use;

[0048] The second org...

Embodiment 3

[0055] 1. Obtaining the primary extract of QJZ

[0056] 1. Crushing:

[0057] Take Qianjinzi as a raw material, put it into a pulverizer for pulverization.

[0058] 2. Organic reagent extraction:

[0059] The stephenia powder was extracted with organic reagents, three consecutive extractions, each extraction time was 6h (heated to 60 degrees, and then heated for 6h). specific:

[0060] The first organic reagent extraction: add 2.5 kg of Stephania chinensis powder to 20 L of organic reagent, the organic reagent is ethyl acetate, stir well until the material liquid is uniform and there are no obvious lumps, turn on the water bath, extract for 6 hours, after the extraction is completed, collect the The supernatant was filtered with filter paper, and the supernatant was concentrated in a rotary evaporator and then transferred to a constant temperature blast drying oven at 60°C for drying to obtain the initial QJZ extract, which was precipitated for use;

[0061] The second org...

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Abstract

The invention relates to a preparation method of a phorbol ester compound Euphorbia Factor L2. A two-dimensional liquid chromatographic technology is adopted to extract Euphorbia Factor L2 from leptochloa chinensis, through reasonable selection of a chromatographic column, a dissolved solution, a mobile phase and the like, optimization of technical conditions such as the flow velocity, the elution mode, the collection section and the like and the orthogonality of the first dimension and the second dimension, complementary separation is realized, so that the whole separation and purification method is practicable, the operability is high, and the purity of the obtained Euphorbia Factor L2 is higher than 98% at most.

Description

technical field [0001] The invention relates to the field of compound production, in particular to a preparation method of a diterpene alcohol ester compound euphorbia factor L2. Background technique [0002] Qianjinzi is the dried and mature seed of Euphorbia lathyris, a plant of the Euphorbia family, which is one of the traditional Chinese medicinal materials in my country. Fructus Qianjinzi is warm in nature, pungent in taste, and slightly poisonous. Its main functions are to expel water to reduce swelling and eliminate blood stasis. , warts. Euphorbia Factor L2 (Euphorbia Factor L2) is a diterpene alcohol ester compound with the molecular formula C 38 h 42 o 9 ,, The molecular weight is 642.283, and its structure is as follows: [0003] [0004] At present, the purification of Euphorbia FactorL2 mainly adopts conventional column chromatography, that is, the method of combining silica gel column chromatography and crystallization, which has a long production cycle...

Claims

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Application Information

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IPC IPC(8): C07C69/78C07C67/48C07C67/56
CPCC07C67/48C07C67/56C07C2602/32C07D213/80C07D213/803C07C69/78
Inventor 张耀洲杨珊珊
Owner TIANJIN YAOYU BIOLOGICAL TECH
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