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Monomeric 7-ethyoxyl ganoderic acid O and separating and purifying method of monomeric 7-ethyoxyl ganoderic acid T thereof

An ethoxylated ganoderma lucidum acid, separation and purification technology, applied in chemical instruments and methods, organic chemistry, steroids and other directions, can solve the problems of high processing temperature, enrichment of impurities, unfavorable stability of biological products, etc., to achieve convenient promotion, Easy-to-operate effects

Active Publication Date: 2010-03-17
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, cold crystallization, vacuum and evaporative crystallization are the main methods of crystallization process. In comparison, vacuum and evaporative crystallization are easy to enrich impurities in the process of concentration, and high processing temperature is also detrimental to the stability of biological products.

Method used

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  • Monomeric 7-ethyoxyl ganoderic acid O and separating and purifying method of monomeric 7-ethyoxyl ganoderic acid T thereof
  • Monomeric 7-ethyoxyl ganoderic acid O and separating and purifying method of monomeric 7-ethyoxyl ganoderic acid T thereof
  • Monomeric 7-ethyoxyl ganoderic acid O and separating and purifying method of monomeric 7-ethyoxyl ganoderic acid T thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] 1. Weigh 100g of dry cell powder obtained from the fermentation of Ganoderma lucidum mycelium, add 2L of chloroform, extract by ultrasonic for 30 minutes, extract 5 times, filter, and rotary evaporate to obtain 7.3g of extract-like substance, and analyze it by high performance liquid chromatography as follows: figure 1 ).

[0055] 2. Dissolve the above-mentioned extract-like substance in 25mL of ether, purify and separate by filling a well-balanced normal-pressure silica gel column in advance, fill with 200g of dry silica gel, the particle size is 200-300 mesh, and the column diameter ratio is 1:10. The diethyl ether of % petroleum ether was used as flow elution, the column volume was about 300 mL, the flow rate was 5 mL / min (full flow rate), and each fraction was collected by an automatic collector. The corresponding components were combined and evaporated to dryness to obtain 3.1 g of solid, which was analyzed by high performance liquid chromatography as figure 2 sh...

Embodiment 2

[0060] 1. Weigh 100g of dry cell powder obtained from the fermentation of Ganoderma lucidum mycelium, add 2L of chloroform, extract by ultrasonic for 30 minutes, extract 3 times, filter, and rotary evaporate to obtain 7.2g of extract-like substance, and analyze it by high performance liquid chromatography as follows: figure 1 shown).

[0061] 2. Dissolve the above-mentioned extract-like substance in 25mL of ether, purify and separate by filling a well-balanced normal-pressure silica gel column in advance, fill with 200g of dry silica gel, the particle size is 200-300 mesh, and the column diameter ratio is 1:10. The diethyl ether of % petroleum ether was used as flow elution, the column volume was about 300 mL, the flow rate was 5 mL / min (full flow rate), and each fraction was collected by an automatic collector. The corresponding components were combined and evaporated to dryness to give 3.1 g of a solid.

[0062] 3. After adding 200mL ether to dissolve the resulting solid, p...

Embodiment 3

[0066] 1. Weigh 100g of dry cell powder obtained from the fermentation of Ganoderma lucidum mycelium, add 2L of chloroform, ultrasonically extract for 30 minutes, extract twice, filter, and rotary evaporate to obtain 7.0g of extract-like substance. HPLC analysis is as follows: figure 1 shown.

[0067] 2. Dissolve the above-mentioned extract-like substance in 25mL of ether, purify and separate by filling a well-balanced normal-pressure silica gel column in advance, fill with 200g of dry silica gel, the particle size is 200-300 mesh, and the column diameter ratio is 1:10. The diethyl ether of % petroleum ether was used as flow elution, the column volume was about 300 mL, the flow rate was 5 mL / min (full flow rate), and each fraction was collected by an automatic collector. The corresponding components were combined and evaporated to dryness to give 3.0 g of a solid.

[0068] 3. After adding 30 mL of ether to dissolve the resulting solid, place it in a crystallizer at -20°C for ...

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Abstract

The invention relates to a monomeric 7-ethyoxyl ganoderic acid O and a separating and purifying method of a monomeric 7-ethyoxyl ganoderic acid T thereof, belonging to the technical field of extraction of organic matters. The separating and purifying method comprises the following steps: preparing dried thallus extract, screening components containing 7-ethyoxyl ganoderic acid O strips, carrying out crystallization treatment, and preparing extract crystal; using reverse liquid-phase chromatogram to analyze crystal purity of ganoderic acid crystal; and using methanol solution to dissolve the ganoderic acid crystal, adding hydrochloric acid in the methanol solution, then placing the obtained solution in an acidolysis reactor for acidolysis treatment to obtain monomeric ganoderic acid crude solution, and finally crystallizing after rotary evaporation treatment and obtaining the ganoderic acid T. The invention can directly obtain ganoderic acid T monomer with the purity of more than 98 percent or 7-ethyoxyl ganoderic acid O with the purity of more than 95 percent, has easy operation and convenient promotion and can lays solid foundation for development and production of relevant drugsof the monomeric ganoderic acid in future.

Description

technical field [0001] The invention relates to a method in the technical field of organic matter purification, in particular to a method for separating and purifying monomeric 7-ethoxyganoderic acid O and monomeric ganoderma acid T. Background technique [0002] Ganoderma lucidum, as a precious medicinal material, has a long history of medicinal use in China and Southeast Asia. Modern medical research shows that Ganoderma acid is one of the important active ingredients of Ganoderma lucidum, which has pharmacological functions such as anti-cancer, anti-HIV virus, and anti-inflammatory response (Acta.Pharmacol.Sin., 25(11), 1387-1395, 2004 Most of the previous studies used Ganoderma lucidum extract (i.e. Ganoderma acid mixture) to study its anticancer activity, so it was difficult to really clarify the pharmacological mechanism of Ganoderma acid. In the past five years, with the research progress in related fields of biotechnology, Several research groups in the world have b...

Claims

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Application Information

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IPC IPC(8): C07J9/00C07J75/00
Inventor 钟建江王家乐李英波
Owner SHANGHAI JIAO TONG UNIV
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