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Method for Rapid Separation and Purification of Monomer Compounds from Yemachai

A technology for separation and purification of compounds, applied in the field of natural medicinal chemistry, can solve the problems of complex operation, large sample loss, large solvent consumption, etc., and achieve the effect of good reproducibility and easy operation.

Inactive Publication Date: 2016-01-20
HUAIYIN TEACHERS COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Most of the above methods require repeated column chromatography, complicated operation, long time consumption, large solvent consumption, and large sample loss

Method used

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  • Method for Rapid Separation and Purification of Monomer Compounds from Yemachai
  • Method for Rapid Separation and Purification of Monomer Compounds from Yemachai
  • Method for Rapid Separation and Purification of Monomer Compounds from Yemachai

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: Take 10.0 kg of dry Ye Ma Zhui, soak it with 100 L of ethanol with a volume concentration of 95% at room temperature for 3 days after crushing, filter, and soak the filter residue 4 times; boil the dregs with 80 L of water for 30 minutes, filter and collect the filtrate, The filter residue was repeatedly decocted 3 times, and the filtrate was combined and concentrated in vacuo to obtain the extract of Yemachai; using chloroform-methanol-water (V:V:V=8:7:3) as the solvent system, the flow rate of the mobile phase (lower phase) was 2mL / min, the rotation speed of the separation column is 900rpm, and the upper phase is the stationary phase. HSCCC separation is carried out on the extract of Yemachai, and the ultraviolet detector is monitored online to collect the target components. The fractions are concentrated and dried under reduced pressure to obtain the corresponding high-purity compounds.

[0018] through 1 H-NMR, 13 C-NMR identification shows that the obta...

Embodiment 2

[0019] Example 2: Take 1.0 kg of dried Yemachai, soak it in 12L of ethanol with a volume concentration of 90% at room temperature for 2 days after crushing, filter, and soak the filter residue three times; boil the dregs with 10L of water for 1 hour, filter and collect the filtrate, The filter residue was repeatedly decocted twice, the filtrate was combined and concentrated in vacuo to obtain the extract of Yemachai; using chloroform-methanol-water (V:V:V=4:3:2) as the solvent system, the flow rate of the mobile phase (lower phase) was 3mL / min, the rotation speed of the separation column is 700rpm, and the upper phase is a stationary phase. HSCCC separation is carried out on the extract of Yemachai, and the ultraviolet detector is monitored online to collect the target components. The fractions are concentrated and dried under reduced pressure to obtain the corresponding high-purity compounds.

[0020] through 1 H-NMR, 13 C-NMR identification shows that the obtained monomer c...

Embodiment 3

[0021] Example 3: Take 500g of dried Yemachai, soak it in 4L of ethanol with a volume concentration of 80% at room temperature for 3 days after crushing, filter, and soak the filter residue three times; boil the dregs with 2.5L of water for 30min, filter and collect the filtrate, The filter residue was repeatedly decocted 3 times, and the filtrate was combined and concentrated in vacuo to obtain the extract of Yemachai; with chloroform-methanol-water (V:V:V=8:5:2) as the solvent system, the flow rate of the mobile phase (lower phase) was 1mL / min, the rotation speed of the separation column is 800rpm, and the upper phase is the stationary phase. The HSCCC separation of the extract of Yemachai is carried out, and the ultraviolet detector is monitored online to collect the target components. The fractions are concentrated and dried under reduced pressure to obtain the corresponding high-purity compounds.

[0022] through 1 H-NMR, 13 C-NMR identification, the obtained monomer com...

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Abstract

The invention discloses a method for rapidly separating and purifying monomeric compounds from Yemachai, which comprises the following steps: taking dried and crushed Yemachai medicinal materials, adding them to ethanol solution for heating under reflux or extracting at normal temperature, removing pigments and other components, and regenerating medicinal residues. Decoct with water, decoct and concentrate under reduced pressure to obtain Yemachai extract; the extract is then separated by high-speed countercurrent chromatography, and the corresponding peak components are collected according to the chromatogram, concentrated and dried under reduced pressure to obtain high-purity uridine and thymine , adenine and uracil. The method has the advantages of high efficiency, simple operation, large preparation amount, and good popularization and use value.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, and in particular relates to a method for rapidly separating and purifying uridine, thymine, adenine and uracil from the traditional Chinese medicine Yemachai. Background technique [0002] Yemachai, also known as Baiguding, Huabivorous, etc., is a plant of the genus Eupatorium in the family Asteraceae. Eupatorium lindleyanum DC.) dry aerial parts. Traditional Chinese medicine believes that wild horses are bitter in taste and flat in nature. Overwork cough, hematemesis and hemoptysis and other diseases. [0003] There is no literature report on the method of separating and purifying uridine, thymine, adenine and uracil from Yemachai. The existing literature reports that the method of separating and purifying uridine, thymine, adenine and uracil from other Chinese herbal medicines often adopts column chromatography. Zou Zhengrong et al [Research on the chemical constituents of Haitia...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H19/067C07H1/08C07D239/54C07D473/34
Inventor 鄢贵龙纪丽莲罗玉明汪伟韩明海
Owner HUAIYIN TEACHERS COLLEGE
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