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A method for separating and preparing verbascoside and mongoside from Budisma japonica

A technology for verbascoside and mongoside, which is applied in the field of rapid separation and preparation of high-purity verbascoside and mongoside, can solve the problems related to methods for obtaining mongoside monomers, etc., and achieve high yield, simple method and high content high effect

Active Publication Date: 2022-02-18
CHINA PHARM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Although there have been Chinese patent reports on the method of extracting fenugreek from Budisma japonica, Chinese patent CN201610254587.8 is a method for extracting japonica japonica from Budisma japonica by ASE method, this method only reports the extraction of japonica japonica from Budisma japonica The method of glucoside does not mention the related method of obtaining mongoside monomer
At the same time, there is no patent report on the preparation of verbascoside from Budisma japonica

Method used

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  • A method for separating and preparing verbascoside and mongoside from Budisma japonica
  • A method for separating and preparing verbascoside and mongoside from Budisma japonica
  • A method for separating and preparing verbascoside and mongoside from Budisma japonica

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Embodiment 1

[0029] Example 1 A method for rapidly separating and preparing high-purity verbascoside and mongoside from Budisma japonica

[0030] (1) Take 50g of Budisma japonica, crush it, extract it twice with 750ml of 60% ethanol solution under reflux at 80°C, each time for 1h, combine the extracts, filter, concentrate under reduced pressure until there is no alcohol smell, and dry to obtain Buddlebags extract 17.9g.

[0031] (2) The extract obtained in step (1) is prepared and purified by high-speed countercurrent chromatography. In the solvent system of ethyl acetate-n-butanol-water (5:0.8:5, v / v / v), the upper phase is the stationary phase and the lower phase is the mobile phase. The rotation speed of the chromatograph is 900rpm, the flow rate of the mobile phase is 2ml / min, the column temperature is 30°C, and the detection wavelength is 313nm. According to HPLC detection, the solvent was evaporated to dryness to obtain 834 mg of verbascoside, with a purity of ≥96.2%; 457 mg of mong...

Embodiment 2

[0035] Example 2 A method for rapidly separating and preparing high-purity mongoside and verbascoside from Budisma japonica

[0036] (1) Take 50g of Budisma japonica, crush it, extract it twice with 1000ml of 60% ethanol solution under reflux at 80°C, each time for 1h, combine the extracts, filter, concentrate under reduced pressure until there is no alcohol smell, and dry to obtain Budhimonica extract 16.7g.

[0037] (2) The extract obtained in step (1) is prepared and purified by high-speed countercurrent chromatography. In the solvent system of ethyl acetate-n-butanol-water (5:0.8:5, v / v / v), the upper phase is the stationary phase and the lower phase is the mobile phase. The rotation speed of the chromatograph is 900rpm, the flow rate of the mobile phase is 2ml / min, the column temperature is 30°C, and the detection wavelength is 313nm. After HPLC detection, the solvent was evaporated to dryness to obtain 789 mg of verbascoside, with a purity of ≥97.3%; and 436 mg of mongo...

Embodiment 3

[0038] Example 3 A method for rapidly separating and preparing high-purity mongoside and verbascoside from Budisma japonica

[0039] (1) Take 50g of Budisma japonica, crush it, extract it twice with 1000ml of 60% ethanol solution under reflux at 80°C, each time for 1h, combine the extracts, filter, concentrate under reduced pressure until there is no alcohol smell, and dry to obtain Budhimonica extract 17.1g.

[0040] (2) The extract obtained in step (1) is prepared and purified by high-speed countercurrent chromatography. In the solvent system of ethyl acetate-n-butanol-water (5:0.8:5, v / v / v), the upper phase is the stationary phase and the lower phase is the mobile phase. The rotation speed of the chromatograph is 900rpm, the flow rate of the mobile phase is 2ml / min, the column temperature is 30°C, and the detection wavelength is 313nm. According to HPLC detection, the solvent was evaporated to dryness to obtain 805 mg of verbascoside, with a purity of ≥96.7%; 442 mg of mo...

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Abstract

The invention relates to a method for rapidly separating and preparing high-purity verbascoside and mongoside from Budhimonica japonica. The extraction method mainly comprises the steps of drying and pulverizing the flower buds as raw materials, extracting them with alcohol solution, recovering the alcohol solution under reduced pressure, and obtaining the flower buds extract. No special treatment is required for the extract of Budisma japonica, and it can be directly separated and purified by high-speed countercurrent chromatography to obtain high-purity verbascoside and mongoside. The invention is simple and reasonable, the final product has high purity, and can be widely used in medicine and sanitation industries.

Description

technical field [0001] The invention relates to a method for rapidly separating and preparing high-purity verbascoside and mongoside. The main processes include alcohol extraction and high-speed countercurrent chromatographic separation. Background technique [0002] Buddleja officinalis Maxim is the dried flower buds and inflorescences of Buddleja officinalis Maxim. Also known as Menghua, rice soup flower, sheep's ear, Xiaojin flower, chicken bone flower, dyed rice flower, etc., it is mainly distributed in the southwest and south-central regions of my country, and the wild resources are very rich. Mimenghua was first recorded in "Kaibao Materia Medica". It is a traditional ophthalmic medicine. The 2015 edition of the "Pharmacopoeia of the People's Republic of China" stipulates that the flower is mainly used for the treatment of red eyes, swelling and pain, tearful eyesight, eye pannus, liver deficiency, dark eyes, dim vision and other diseases. It is an effective treatment...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/18C07H17/07C07H1/08
Inventor 秦民坚谢国勇王飒秦晓颖张翔吴刚
Owner CHINA PHARM UNIV
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