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Method for quickly separating and purifying monomeric compound from lindley eupatorium

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

Inactive Publication Date: 2014-08-06
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 quickly separating and purifying monomeric compound from lindley eupatorium
  • Method for quickly separating and purifying monomeric compound from lindley eupatorium
  • Method for quickly separating and purifying monomeric compound from lindley eupatorium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0018] through 1 H-NMR, 13 C-NMR identification shows that the obtained monomer compounds ar...

Embodiment 2

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

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

Embodiment 3

[0021] Example 3: Take 500 g of dried Ye Ma Zhui, soak it in 4 L 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 2.5 L of water for 30 min, filter and dry Collect the filtrate, decoct the filter residue three times, combine the filtrates and concentrate in vacuo to obtain the extract of Yemachai; use chloroform-methanol-water (V:V:V=8:5:2) as the solvent system, and the mobile phase (lower phase ) with a flow rate of 1 mL / min, a separation column rotation speed of 800 rpm, and a stationary phase as the upper phase. The HSCCC separation of the extract of Yemachai was carried out, and the ultraviolet detector was monitored online to collect the target components. The fractions were concentrated and dried under reduced pressure to obtain the corresponding high Purity compound.

[0022] through 1 H-NMR, 13 C-NMR identification, gained monomer compound is respectively...

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Abstract

The invention discloses a method for quickly separating and purifying a monomeric compound from lindley eupatorium. The method comprises the following steps: taking dried and crushed lindley eupatorium drugs, adding the dried and crushed lindley eupatorium drugs to an ethanol solution to carry out heating reflux or normal-temperature digestion; removing ingredients such as a pigment, decocting dregs by using water, and concentrating a decoction solution in vacuum, so as to obtain a lindley eupatorium extract; separating the extract by using a high-speed counter current chromatograph, collecting a corresponding peak component according to a chromatogram map, and concentrating and drying in vacuum, so as to obtain high-purity uridine, thymine, adenine and uracil. The method is high in efficiency, simple to operate, and large in preparation quantity, and has good popularization and application 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 Haiti...

Claims

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Application Information

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Patent Type & Authority Applications(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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