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Method for extracting scopoletin from erycibe obtusifolia benth

A technology of scopolide and terpenoids, which is applied in the field of extracting scopolide, can solve the problems of artificial synthesis method, such as low yield, insufficient extraction, and long use time, and achieves low production cost, good degreasing effect, and difficult residue. Effect

Inactive Publication Date: 2011-04-06
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The extraction is not thorough enough and the utilization rate is low
Yang Yuzhong et al. "Determining the Content of Scopoletin in Ding Gong Teng by HPLC" mentioned the simple research results on the extraction of low-carbon alcohol solution, reflecting that the extraction time by solvent reflux alone is very long
However, artificial synthesis methods generally have problems such as low yield, high cost, and rare raw materials, such as the three methods of synthesizing scopoletin mentioned in "Research Progress of Natural Product Scopoletin" by Wei Lijuan et al.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Take 2 kg of Dinggongia glabrata (scopolamine content 0.19%), grind it to 60 mesh, add 4 L of petroleum ether to degrease for 4 hours and repeat once to obtain a degreased material. Add 16L of 70% ethanol, ultrasonically extract at room temperature for 30min, extract under reduced pressure to recover ethanol, concentrate to extract 74.2g, disperse the extract with 230ml of 5% sodium hydroxide solution, filter and add hydrochloric acid to the filtrate to acidify to pH6, concentrate To extract 52.6g. The acidified extract was extracted with 1.2L of chloroform, filtered, concentrated to recover chloroform, evaporated to dryness to obtain a crude product, crystallized twice with 75% ethanol, filtered out and dried at low temperature to obtain 3.3g of the product with a content of 96.2%.

Embodiment 2

[0034] Take 2 kg of Ding Gong Teng (scopolamine content 0.2%), grind it to 40 mesh, add 3 L of petroleum ether to degrease for 3 hours and repeat once to obtain a degreased material. Add 18L of 70% ethanol, ultrasonically extract at room temperature for 40 minutes, extract the extract under reduced pressure to recover ethanol, and concentrate to obtain 76.3g of extract. The extracted extract was dispersed with 320ml of 5% sodium hydroxide solution, after filtration, the filtrate was acidified to pH6 with hydrochloric acid, and concentrated to 43.8g of extract. The acidified extract was extracted with 1L of chloroform, filtered, concentrated to recover chloroform, evaporated to dryness to obtain a crude product, added 85% ethanol for crystallization three times, filtered out and dried at low temperature to obtain 3.7g of the product with a content of 97.4%.

Embodiment 3

[0036] Take 2 kg of Dinggongia glabrata (scopolamine content 0.21%), grind it to 80 mesh, add 4 L of petroleum ether to degrease for 3 hours and repeat once to obtain a degreased material. Add 20L of 70% ethanol, ultrasonically extract at room temperature for 50min, extract under reduced pressure to recover ethanol, concentrate to extract 78.3g, disperse the extract with 390ml of 5% sodium bicarbonate solution, filter and add hydrochloric acid to the filtrate to acidify to pH5, concentrate To extract 46.8g. The acidified extract was extracted with 1.3L chloroform, filtered, concentrated to recover chloroform, evaporated to dryness to obtain a crude product, crystallized twice with 90% ethanol, filtered and dried at low temperature to obtain 3.5g product with a content of 96.7%.

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Abstract

The invention relates to a method for extracting scopoletin from erycibe obtusifolia benth, which comprises the following steps of: crushing the erycibe obtusifolia benth serving as a raw material to 40 to 80 meshes, degreasing the material by using petroleum ether, adding 70 percent ethanol into the material to perform ultrasonic extraction for 30 to 60 minutes, concentrating the extracted substance to obtain extract, dissolving the extract in thin alkali, filtering the solution, adding acid into the filtrate for reduction, continuously concentrating the filtrate to obtain acidified extract, adding chloroform into the acidified extract for extraction, reclaiming the chloroform, and re-crystallizing to obtain a product by using 75 to 90 percent ethanol. The method for producing the product has thorough extraction and little pollution and can be used for large-scale production.

Description

Technical field: [0001] The invention relates to a method for extracting scopoletin from Dinggongteng vine, in particular to a method for preparing scopoletin by ultrasonic extraction, acid-base method purification and recrystallization. Background technique: [0002] Erycibe obtusifolia Benth. is a plant of the genus Erycibe obtusifolia in the family Convolvulaceae, with slightly hairy twigs. The branches and leaves are luxuriant and the leaves are emerald green. Leaves ovate to oblong, with 5-8 lateral veins on each side, slightly protruding ventral surface. It blooms in summer and autumn, the flowers are yellow and white, and the corolla is 5 deeply lobed. Berries subglobose, glabrous. Distributed in Guangdong, Hainan, Guangxi, and Yunnan in China; northern Vietnam. Produced in moist dense forests in valleys, roadside bushes can be seen. The stems and twigs are used as medicine (soaked in wine) to cure rheumatism. [0003] Nature and flavor: warm in nature, pungent ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/16
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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