Method for separating and preparing anti-tumor components ganoderic acid C1 and ganoderic acid F

Abstract

The invention discloses a method for separating and preparing anti-tumor components ganoderic acid C1 and ganoderic acid F, which comprises the following steps: (1) primarily enriching and purifying the alcohol extract of lucid ganoderma by use of macroporous resin, and separating a ganoderic acid part with purity of 30-60% from the alcohol extract of lucid ganoderma; (2) separating the separated ganoderic acid part through high-speed counter-current chromatography to obtain ganoderic acid with relatively high purity, wherein a solvent system consists of petroleum ether, ethyl acetate, methanol and water at a volume ratio of 5:(3-7):(1-6):(4-9); the upper phase of the solvent is a stationary phase, and the lower phase is a mobile phase; a sample is dissolved with the lower phase solution and fed; the flow velocity of the stationary phase is 10-20mL / min, the flow velocity of the mobile phase is 1.5-3mL / min, and the rotation speed of the host is 600-1,000rpm; the separated object is collected by an automatic fraction collector, and one fraction is collected from every 4-10mL; (3) analyzing and detecting the components of the liquid collected by each test tube by high performance liquid chromatography, collecting, concentrating and drying according to different components, and separating to obtain ganoderic acid C1 and ganoderic acid F with purity up to 95%. The method has the characteristics of high efficiency, high speed, large separation quantity, high recovery rate, solvent saving and the like.

Description

technical field [0001] The invention relates to a method for separating and preparing high-purity anti-tumor components ganoderma acid C1 and ganoderma acid F from ethanol extracts of ganoderma lucidum, in particular to a combination of macroporous resin chromatography and high-speed countercurrent chromatography, A method for separating and preparing high-purity anti-tumor components ganoderma acid C1 and ganoderma acid F. Background technique [0002] Ganoderma lucidum, also known as Ruicao, Wannian mushroom, etc., is a large medicinal fungus belonging to the genus Ganoderma of the family Polyporaceae, including Ganoderma lucidum (Levss. ex Fr.) Karst. and Ganoderma sinense Zhao. Xu Dry fruiting bodies of et zhang. It has the effects of invigorating the middle and Qi, nourishing yin and strengthening, strengthening the body, prolonging life, etc., and it has been listed as top grade in medical books of all dynasties. Ganoderma lucidum triterpenoids are one of the importa...

AI Technical Summary

Problems solved by technology

Since supercritical carbon dioxide is a non-polar solvent, it is suitable for extracting non-polar or low-polar components, but it is difficult to extract relatively polar components such as ganoderma acid. Therefore, the extraction rate of ganoderma acid with supercritical carbon dioxide is not only low, More importantly, the non-polar and low-polar components in Ganoderma lucidum are preferentially extracted, which greatly reduces the purity of Ganoderma acid in the extract. Therefore, the purity of Ganoderma acid obtained by this method is generally lower than 20%. One of dozens of ganoderma acids contained, so ganoderma acid A is less than 10% in this extract

Due to the low purity of the sample and many impurities, and without further purification, it was directly separated by high-speed countercurrent to obtain 95% high-purity ganoderma acid A, which greatly increased the amount of toxic solvents such as methanol and chloroform used in high-speed countercurrent separation, and also brought environmental pollution. Aspects

[0004] In the Chinese patent CN 101671383B, 7-ethoxyganoderic acid O and ganoderma acid T were prepared by silica gel column chromatography combined with crystallization method, although the purity can be obtained Ganoderma acid monomer, but its separation and purification methods have certain limitations

Because silica gel column chromatography requires the use of toxic solvents such as methanol and chloroform, and silica gel cannot be reused, it will be thrown away once it is used up, which will easily cause waste of resources and environmental pollution; and in this patent, due to the purity of the sample after preliminary purification of silica gel Not enough, so it is necessary to add high-purity crushed ganoderma acid crystals to induce crystallization during the crystallization process. These high-purity crushed ganoderma acid crystals (high purity, equivalent to the reference substance) are generally expensive and difficult to prepare, which also increases the cost of the test

[0005] In addition to the above patents, there is currently no combination of macroporous resin chromatography and high-speed countercurrent chromatography to separate and prepare high-purity anti-tumor components Ganoderma acid C1 and Ganoderma lucidum Sour F Method

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