Extraction method of alkannin

An extraction method and technology for shikonin, applied in the directions of organic chemistry, quinone separation/purification, etc., can solve the problems of low utilization rate of raw materials, unfavorable for large-scale production, and low yield.

Active Publication Date: 2013-10-30
SICHUAN ACAD OF CHINESE MEDICINE SCI
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  • Summary
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  • Application Information

AI Technical Summary

Problems solved by technology

CN1206726A introduces to soak comfrey roots directly at 30-35°C with n-hexane, petroleum ether, and solvent oil, and then concentrate under reduced pressure to obtain a black-red ointment, which is then made into an aqueous solution with Tween 80, and then adsorbed with dextrin Finally, spray drying to make water-solu

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take 1 kg of comfrey root powder, according to the volume / weight ratio of petroleum ether to comfrey powder (L / kg) 6 : 1 Reflux extraction with petroleum ether (60~90°C) for 4 times, each time for 1 hour, and filter. Part of the solvent is recovered from the extract. Extract with 1.5M NaOH solution, the volume ratio of alkali solution to petroleum ether extract solution is 1 : 1. Alkaline extraction solution was acidified with hydrochloric acid to pH 1~2, precipitates were precipitated, left to stand, filtered with suction, washed with distilled water until neutral, and dried under reduced pressure at 55°C to obtain 29.3g of shikonin extract with a purity of 93.8%. 2.93%.

Embodiment 2

[0022] Take 1kg of comfrey root powder, according to the volume-to-weight ratio of solvent and comfrey powder (L / kg) 10 : 1. Reflux extraction with n-hexane for 3 times, each time for 1 hour, and filter. Part of the solvent is recovered from the extract. Extract with 0.6M NaOH solution, the volume ratio of alkali solution to petroleum ether extract solution is 1 : 1. Stand still and separate the alkali layer solution. Acidify the alkali solution extract with dilute sulfuric acid to pH 1~2, there is a precipitate, stand still, filter with suction, wash the precipitate with distilled water until neutral, and dry under reduced pressure at 50°C to obtain 31g of shikonin extract with a purity of 75.5%. The yield is 3.1%.

Embodiment 3

[0024] Take 700 g of comfrey root powder, extract with cyclohexane for 4 times under reflux according to the volume-to-weight ratio (L / kg) of solvent to comfrey powder (L / kg) 4 times, each time for 1 hour, and filter. Part of the solvent is recovered from the extract. Extract with 2.5M NaOH solution, the volume ratio of alkali solution to petroleum ether extract solution is 1 : 1. Stand still and separate the alkali layer solution. Acidify the alkali solution extract with hydrochloric acid to pH 1~2, a precipitate precipitates out, let stand, filter with suction, wash the precipitate with distilled water until neutral, and dry under reduced pressure at 50°C to obtain 14.35 g of shikonin extract with a purity of 82.5%. The yield is 2.05%.

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Abstract

The invention relates to an extraction method of alkannin. In the extraction method, after extracting lithospermum with organic menstruum, aqueous alkali is used for processing. The method is characterized in that after the lithospermum is fully extracted with nonpolar organic menstruum in a backflow mode, aqueous alkali containing sodium hydroxide or potassium hydroxide with the concentration of 0.6-5.5M is used for fully leaching an organic solution after the fully extracting, then the pH value of aqueous alkali extraction solution is acidized to be smaller than or equal to 2, then the lithospermum is fully precipitated and collected. By using the extraction method in the invention, the lithospermum with high purity and yield can be obtained and can be applied to the commercial process.

Description

technical field [0001] The present invention relates to a method for extracting shikonin from raw materials containing shikonin and shikonaquinones, especially shikonin root. Background technique [0002] Comfrey is not only a natural plant but also a raw material of Chinese medicinal materials. The comfrey recorded in the Chinese Pharmacopoeia 2010 edition is the dried root of Arnebia euchroma (Royle) Johnst. in Xinjiang or Arnebia guttala Bugede in Inner Mongolia. The main chemical constituents in comfrey plants are mainly shikonadhiquinones, phenolic acids, alkaloids, phenols and benzoquinones, triterpene acids and sterols, flavonoids and polysaccharides. Among them, the most important compounds in comfrey root are shikonaquinone compounds, mainly including shikonin, acetylshikonin, β,β-dimethylacryloylshikonin, isovalerylshikonin, isobutyryl purple Grass and so on. Comfrey is widely used in the food industry, cosmetics industry, and pharmaceutical industry due to its ...

Claims

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Application Information

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IPC IPC(8): C07C50/32C07C46/10
Inventor 潘晓鹃王芳唐雪梅沈立王聪周建
Owner SICHUAN ACAD OF CHINESE MEDICINE SCI
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