Process for preparing thermopsis lanceolate total alkaloids and several high-purity medicinal substances

A technology of Huanghua lanceolate and total alkaloids is applied in the directions of medical preparations containing active ingredients, antitumor drugs, drug combinations, etc. Use of acids, bases and organic solvents, the effects of improving stability and safety in production and operation

Inactive Publication Date: 2012-02-15
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method disclosed in Chinese Patent Application No. 200910023485.5 is to pulverize the seeds of lanceolus Huanghua, extract and concentrate to obtain the extract, extract the extract with an organic solvent, back-extract the acid aqueous solution, purify the extraction solvent, and simultaneously obtain the acid containing Huang Hua alkali. Aqueous solution, this acid aqueous solution is alkalized by adding alkaline reagents, crystallized, and recrystallized to obtain chrysanthemum; the extracted extract solution is alkalized and then extracted with an organic solvent, concentrated, crystallized, and recrystallized to obtain pure gorse Alkali, this method uses a large amount of acid-base solution, which is not conducive to the stability of the components, and uses strong toxic solvents such as benzene, which is unsafe to operate
The method disclosed in Chinese Patent Application No. 201010240158.8 is to obtain the total alkaloids through extraction, concentration, acid water acidification, alkalization, and organic solvent extraction. The total alkaloids are dissolved in water and extracted with organic solvents to obtain cytisine. The method Cytisine can be obtained only by extracting from total alkaloids with organic solvents, which is not easy to achieve in actual production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take lanceolus Huanghua leaves and grind them, add 5 times the amount of hydrochloric acid aqueous solution with pH 1.0 to extract dynamically 3 times, each time for 1.5h, combine the extracts, concentrate the extracts, pass through 732 strong acid cation exchange resin, and wash with water to the washing solution If it is neutral, add ammonia water to the resin to make it alkaline, free the alkaloid, elute with 85% ethanol, collect the ethanol eluate, concentrate under reduced pressure until there is no alcohol smell, and pass through the X-5 macroporous adsorption resin column , first eluted with water, then eluted with 60% ethanol, collected the eluate, concentrated and dried to obtain the total alkaloid extract.

[0021] Dichloromethane, isopropanol, 0.02M Na 2 HPO 3 Mix, oscillate and shake evenly to make the two phases reach equilibrium, separate after standing and stratifying, the lower phase is the mobile phase, and the upper phase is the stationary phase, resp...

Embodiment 2

[0025] Take lanceolus Huanghua leaves and grind them, add 5 times the amount of sulfuric acid aqueous solution with pH 3.0 to dynamically extract twice, each time for 2 hours, combine the extracts, concentrate the extracts, pass through HZ002 strong acid cation exchange resin, and wash with water until the washing liquid is Neutral, then add ammonia water to the resin to alkalinize, free the alkaloid, elute with 85% ethanol, collect the ethanol eluate, concentrate under reduced pressure until there is no alcohol smell, pass through SIP-1100 macroporous adsorption resin column, First elute with water, then elute with 75% ethanol, collect the eluate, concentrate and dry to obtain the total alkaloid extract.

[0026] Dichloromethane, isopropanol, 0.02M Na 2 HPO 3 Mix, oscillate and shake evenly to make the two phases reach equilibrium, separate after standing and stratifying, the lower phase is the mobile phase, and the upper phase is the stationary phase, respectively degas the...

Embodiment 3

[0030] Take lanceolus Huanghua leaves and grind them, add 5 times the amount of acetic acid aqueous solution with pH 2.6 for dynamic extraction once, each time for 1.5h, combine the extracts, concentrate the extracts, pass through JK006 strong acid cation exchange resin, and wash with water to the washing solution If it is neutral, add ammonia water to the resin to alkalinize it. After freeing the alkaloid, elute it with 80% ethanol, collect the ethanol eluate, concentrate it under reduced pressure until it has no alcohol smell, pass it through a HP20 macroporous adsorption resin column, and first Elute with water, then elute with 50% ethanol, collect the eluate, concentrate and dry to obtain the total alkaloid extract.

[0031] Dichloromethane, isopropanol, 0.02M Na 2 HPO 3 Mix, oscillate and shake evenly to make the two phases reach equilibrium, separate after standing and stratifying, the lower phase is the mobile phase, and the upper phase is the stationary phase, respect...

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Abstract

The invention relates to a process for preparing thermopsis lanceolate total alkaloids and several high-purity medicinal substances, and belongs to the technical field of the extraction of Chinese medicinal active ingredients. The medicinal substances comprise eulexine, thermopsine, sparteine and N-methyl eulexine. In the process, total alkaloids are prepared from thermopsis lanceolate serving as a raw material through acid water extraction, ionic resin adsorption and macroporous resin enrichment, and the total alkaloids are separated and purified by high-speed countercurrent chromatography and preparative liquid chromatography to obtain the high-purity eulexine, thermopsine, sparteine and N-methyl eulexine. The process has the advantages of simplicity, quickness, high repeatability, large preparation amount and the like, and industrialization is easy to realize.

Description

technical field [0001] The invention belongs to the technical field of separation and purification of active components of traditional Chinese medicines, and in particular relates to a preparation process of total alkaloids of lanceolata chinensis and several high-purity medicinal substances. Background technique [0002] Coniferous yellow flower ( Thermopsis lanceolate ), alias Mu Madou, Mongolian "Furday Bagan-Xiri", is a perennial herb belonging to the genus Cassia genus Fabaceae. Distributed in the northeast, north and Shaanxi, Gansu, Qinghai, Ningxia, Sichuan and other provinces and regions, the main chemical components of lanceolus Huanghua are quinolizidine alkaloids, and the total alkaloid content varies greatly due to different parts. The content is the highest, followed by flowers, fruits, leaves, stems, and roots. This type of alkaloid has various pharmacological effects such as anti-cancer, anti-arrhythmia, anti-microbial, anti-ulcer, and increasing white blood ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/48C07D471/18C07D471/22A61P35/00A61P9/06A61P31/00A61P17/02A61P7/00A61P11/16A61P15/18A61P25/00A61P25/28A61P25/02A61P23/00A61P31/10A61P15/04A61P9/04A61P21/00
Inventor 刘东锋郭琴
Owner NANJING ZELANG MEDICAL TECH
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