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Extracting method for drumstick phenanthrene

An extraction method, the technology of phenanthrene, which is applied in the field of separation and purification of phenanthrene by macroporous resin and high-speed countercurrent chromatography, can solve the problems of undiscovered separation of phenanthrene compounds in Dendrobium, and achieve high yield of preparation process Effect

Inactive Publication Date: 2012-08-29
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Drumstick phenanthrene is one of the active ingredients of traditional Chinese medicine isolated from the genus Dendrobium. In the relevant searches of the State Intellectual Property Office and the China Journal Network search, no process research on the extraction and separation of phenanthrene compounds in the genus Dendrobium was found.

Method used

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  • Extracting method for drumstick phenanthrene

Examples

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Comparison scheme
Effect test

Embodiment 1

[0017] Take Dendrobium medicinal materials and grind them, take 10kg and put them into a 200L pilot test extraction tank, add 100L80% ethanol solution to reflux and extract for 2 hours, extract the supernatant, then extract twice under the same conditions, combine the extracts, and concentrate the extracts to a small Volume, to obtain the crude extract, after the crude extract was trans-dissolved with 10 times of 20% ethanol solution, the supernatant was added to a D101 macroporous resin column (column diameter to height ratio 1:7) for adsorption, and the adsorption flow rate was 2.5L / h After the adsorption is completed, it is eluted with water, 30% ethanol, and 80% ethanol in sequence, and the 80% ethanol eluate is collected, and 45 g of medicinal activated carbon for injection is added for decolorization, and the activated carbon is filtered out, and concentrated to 1 / 13 of the original volume to obtain a precipitate Wash the precipitate with petroleum ether to obtain 6.0 g o...

Embodiment 2

[0019] Take Dendrobium medicinal materials and grind them, take 10kg and put them into a 200L pilot test extraction tank, add 120L90% ethanol solution to reflux and extract for 1.5 hours, extract the supernatant, then extract 3 times under the same conditions, combine the extracts, and concentrate the extracts to a small Volume, to obtain the crude extract, after the crude extract was trans-dissolved with 15 times of 20% ethanol solution, the supernatant was added to the AB-8 macroporous resin column (column diameter to height ratio 1:5) for adsorption, and the adsorption flow rate was 3.5L / h, after the adsorption is completed, it is eluted with water, 30% ethanol, and 80% ethanol successively, and the 80% ethanol eluate is collected, and 40.5 g of medicinal activated carbon for injection is added for decolorization, the activated carbon is filtered out, and concentrated to 1 / 12 of the original volume to obtain For the precipitate, wash the precipitate with petroleum ether to ...

Embodiment 3

[0021] Take Dendrobium medicinal materials and grind them, take 10kg and put them into a 200L pilot test extraction tank, add 140L of 70% ethanol solution to reflux and extract for 1.5 hours, extract the supernatant, then extract twice under the same conditions, combine the extracts, and concentrate the extracts to a small Volume, to obtain the crude extract, after the crude extract was trans-dissolved with 8 times of 20% ethanol solution, the supernatant was added to the AB-8 macroporous resin column (column diameter to height ratio 1:6) for adsorption, and the adsorption flow rate was 2.0L / h, after the adsorption is completed, elute with water, 30% ethanol, and 80% ethanol in sequence, collect the 80% ethanol eluate, add 75g of medicinal activated carbon for injection for decolorization, filter out the activated carbon, concentrate to 1 / 10 of the original volume, and obtain a precipitate The precipitate was washed with petroleum ether to obtain 6.4 g of powdery crude product...

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Abstract

The invention relates to an extracting method for drumstick phenanthrene, which comprises the following steps of: crushing dendrobium plant drugs; performing ultrasonic or backflow extraction by taking 70-95% alcohol solution; concentrating the extracting solution, thereby obtaining a crude extract; dissolving the crude extract with 8-20 times of 20% alcohol; taking macroreticular resin from supernate; decolorizing by adding active carbon into eluent injection; filtering the active carbon; concentrating, thereby obtaining precipitate; washing the precipitate with petroleum ether, thereby obtaining crude product; separating and purifying the crude product by adopting a HSCCC (High Speed Counter Current Chromatography) method; and reducing pressure and drying the effluent, thereby obtaining the product. The method is simple in process for producing the drumstick phenanthrene; the purity is high; and the preparation volume is large.

Description

Technical field: [0001] The invention relates to a method for extracting phenanthrene tympani, in particular to a method for separating and purifying phenanthrene chrysanthemum by adopting macroporous resin and high-speed countercurrent chromatography. Background technique: [0002] In recent years, the research on the antitumor activity of bibenzyl and phenanthrene compounds is being highly valued by foreign scholars. 1210 Tubulin aggregation and mitosis, cell lines, a variety of human tumor cell lines such as A-549, MCF-7, HT-29, SKMEL-5, MLM, SK-OV-3, HL-60 all have inhibitory effects. Ma Guoxiang et al. selected liver cancer and Ehrlich ascites cancer as the tumor spectrum, and carried out anti-tumor activity research on the ethanol extract of Dendrobium chrysalis, Erianin, Mao Lanfei, and Drumstick phenanthrene. The results showed that: Each monomer has anti-tumor activity in different degrees. Erianin has the strongest effect on mouse liver cancer, and its tumor inhib...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/23C07C41/36A61K31/09A61P35/00A23L1/29A23L33/00
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司