Method for preparing limonin, composition and application thereof

Abstract

The invention provides a method for preparing a composition comprising high-purity limonin and a medicinal composition which is prepared by the method, has high safety and comprises the high-purity limonin. In the preparation method, the limonin of which the purity is over 98 percent can be obtained under the condition of recrystallization and purification for two times; and the impurities in the limonin do not damage the safety. Moreover, the invention also provides application of the medicinal composition in preparing a medicament for preventing and / or treating the colon cancer or the rectal cancer.

Description

technical field [0001] The invention belongs to the field of herbal medicines (Chinese herbal medicines). Specifically, the invention relates to a method for preparing high-purity limonin and a high-safety pharmaceutical composition containing high-purity limonin. In addition, the present invention also relates to the application of the above pharmaceutical composition in the preparation of medicaments for preventing and / or treating colon cancer or rectal cancer. Background technique [0002] Limomin, also known as evocarptonin, phrysinide, phellodactone, mainly exists in Rutaceae (Rutaceae) and Meliaceae (Meliaceae) plants, such as Citrus aurantium (navel orange, citrus, Among orange) pomelo, etc., the content in the core (seed) is higher, and the content in the peel is less (about 1 / 10,000 to 5 / 100,000). The chemical structure of limonoid is shown below: [0003] [0004] Limonin has anti-cancer, analgesic, anti-inflammatory, lowering cholesterol, inhibiting HIV-1 vir...

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Problems solved by technology

[0005] At present, the preparation method of limonin has been reported in the existing literature, but either the solvent is wasted in the preparation and the extraction rate is low, resulting in high production cost; or the prepared composition (product) has low purity and contains more impurities. Direct use brings great hidden dangers to drug safety, and it is difficult to pass approval for actual industrialization, and further purification is equivalent to increasing the cost of preparation

[0006] Specifically, Chinese Patent Application No. 00106285 discloses a method for extracting limonin from Rutaceae fruits, but the purity of limonin prepared by this method is very low (less than 90%);

[0007] Chinese patent application No. 00130622 discloses a process for extracting medicinal active substances from citrus seeds. However, the purity of limonin prepared by this process is very low. We have found that to obtain high-purity products, it is necessary to pass through silica gel chromatography. Recrystallization steps (much more than 2 times) are frequently used after the column, the extraction rate is low and the cost is high;

[0009] Chinese patent application No. 03118175 discloses a method for simultaneously extracting eight kinds of products such as pectin and naringin from pomelo, but this method will lose a large amount of limonin when debittering through the adsorption resin, resulting in limonin The extraction rate is low, and the other three column separations result in complicated processes and are not suitable for industrialization;

[0012] Chinese patent application No. 200810037312 discloses a process for preparing limonin monomer by industrial chromatography. In this document, the industrial chromatography column is used after crystallization and before recrystallization, and the loss of limonin is relatively large, and our research found that , although the literature claims (and does not provide evidence to prove) that the limonin purity in the product is greater than 98%, 99%, but we repeated its examples and found that the purity is preferably no more than 93%, which cannot reach the Safe purity, if you want to increase the purity, you need to increase the recrystallization process several times;

[0013] Chinese patent application No. 200810046164 discloses a method for separating limonin, evodiamine and evodiamine from Evodia rutaecarpa. However, high-efficiency preparation of liquid phase separation is required, which is not suitable for industrial production (or the cost of industrial production is extremely high), only Suitable for laboratory preparation;

This method uses expensive hexane for degreasing, which is costly and has a low extraction rate

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