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Juncus effususl phenanthrene effective part and preparation method and use thereof

An effective part, the technology of rushes, applied in the field of medicine, can solve the problems of crude extract containing a large amount of impurities, quality control of rushes extract, toxic and side effects, etc., and achieve simple and easy quality control, simple and easy preparation process, and low production cost Effect

Inactive Publication Date: 2015-09-23
BEIJING UNIV OF CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In addition, if the rush is extracted by the existing extraction method, the obtained crude extract contains a large amount of impurities
This situation is not conducive to the quality control of the rush extract, and the existence of a large number of impurities introduces more uncontrollable factors, such as possibly causing some toxic side effects, etc.

Method used

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  • Juncus effususl phenanthrene effective part and preparation method and use thereof
  • Juncus effususl phenanthrene effective part and preparation method and use thereof
  • Juncus effususl phenanthrene effective part and preparation method and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Take 1.5kg of rush stem pith and extract twice with 80% ethanol solution by volume ratio, for the first time reflux extraction with 25 times volume ratio of 80% ethanol solution for 1.5h, and for the second time with 15 times volume ratio Reflux extraction with 80% ethanol solution for 1 h, combine the extracts, concentrate, and dry to obtain 90 g of dry ethanol extract. The ethanol extract was mixed with 3 times the amount of silica gel, ultrasonically extracted twice with 40 times the amount of ethyl acetate, each time for 30 minutes, the extracts were combined, concentrated, and dried to obtain 18 g of dry ethyl acetate crude extract.

[0048] Take 400 mg of the above-mentioned dry ethyl acetate crude extract, dissolve it in methanol, dry mix the sample with 1.2 g of silica gel (60-80 mesh), and load the sample on a silica gel column (a glass column with a diameter of 3 cm and a height of 30 cm is filled with a 60-80 mesh Silica gel 20g), eluting with petroleum ether...

Embodiment 2

[0050] The dry ethyl acetate crude extract was prepared in the same manner as in Example 1.

[0051] Take 209 mg of the above-mentioned dry ethyl acetate crude extract, dissolve it in methanol, dry mix the sample with 0.6 g of silica gel (200-300 mesh), load the sample on a silica gel column (a glass chromatographic column with a diameter of 1.5 cm and a height of 15 cm is filled with 200-300 Mesh silica gel 20g), eluted with petroleum ether: ethyl acetate (5:2), tracked and collected the samples with UV absorption with a fraction collector equipped with a UV detector, and recovered the solvent to obtain the effective part of phenanthrene. UV absorbance is negative. Obtained 46mg of phenanthrene effective fraction and 121mg of negative sample. Measured by the high-performance liquid chromatography of Examples 13 and 14, the content of dehydroeuphorol in the effective parts of phenanthrenes is 59%, and the area ratio of dehydroeuphorol, dehydroeuphorol, urge mol, and phenanthr...

Embodiment 3

[0053] The dry ethyl acetate crude extract was prepared in the same manner as in Example 1.

[0054] Take 236mg of the above-mentioned dry ethyl acetate extract, dissolve it in ethanol, mix the sample with 0.7g silica gel (200-300 mesh), and use a 10g biotage chromatographic column to separate with flash preparative chromatography (Isolera One), mobile phase: petroleum ether: ethyl acetate (5:2) isocratic elution; equilibrium flow rate: 10ml / min, equilibrium volume 15ml; elution flow rate 10ml / min; detection wavelength 270nm, see chromatogram for separation Figure 3A-Figure 3C . Combined at 0-14 minutes to obtain 66 mg of the effective part of phenanthrene, 14-35 minutes and other samples not eluted in the chromatographic column were ultrasonically extracted with ethyl acetate and combined to obtain 117 mg of negative samples. Measured by the high-performance liquid chromatography of Examples 13 and 14, the content of dehydroeuphorol in the effective part of phenanthrene is ...

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Abstract

The present invention relates to a juncus effususl phenanthrene effective part and a preparation method and use thereof in the manufacture of anti-anxiety drugs, the juncus effususl phenanthrene effective part contains more than 50% of effusol, dehydroeffusol, juncus effususl phenol and dehydro juncus effususl phenol, the preparation method comprises the following steps: taking juncus effususl stem medulla, using an ethanol aqueous solution for extraction with refluxing; combining the obtained extract and concentrating, then using ethyl acetate for ultrasound extraction, combining the extract, concentrating and drying the combined extract to obtain a dry ethyl acetate crude extract; and taking the dry ethyl acetate crude extract for silica gel column chromatography or high-speed countercurrent chromatography separation to obtain the juncus effususl phenanthrene effective part.

Description

technical field [0001] The invention relates to the effective part of rush phenanthrene and its preparation method and its application in the preparation of anti-anxiety drugs, belonging to the technical field of medicine. Background technique [0002] Juncus effuses L. is the dry stem marrow of Juncus effuses L., sweet, light and slightly cold. Guixin, lung, small intestine channel. It can clear heart fire and facilitate urination. For upset and insomnia embolism. Rush contains phenanthrenes, flavonoids, terpenes, steroids and volatile oils, among which phenanthrene compounds are one of the main components. In the 1990s, mainly foreign scholars such as Della Greca and Asakawa conducted research on the chemical components and antitumor, cytotoxic, antioxidative, antimicrobial and algicidal activities of rushes. In recent years, Yang Guangzhong, Shan Chengying and other research teams have also begun to devote themselves to the research on the chemical composition and ant...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/88A61P25/22
Inventor 黄建梅李贵云段天璇詹雪艳王杨
Owner BEIJING UNIV OF CHINESE MEDICINE
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