Joint preparation method for euscaphic acid and tormentic acid

A technology for the joint preparation of Potentate acid, applied in steroids, organic chemistry, etc., can solve the problems of no simultaneous preparation of two substances, no patent reports, etc., and achieve high recovery rate and high throughput Large, simple effect of solvent system

Inactive Publication Date: 2012-03-28
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the existing literature, there are relatively few research reports on pollenic acid and rosinic acid, and there is no method for preparing the two substances at the same time, and there are no related patent reports

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 1 kg of Gugongguo medicinal material, grind it, add 10L of 40% ethanol solution to heat reflux extraction twice, combine the extracts, concentrate to low alcohol, and absorb on macroporous resin, first use 2BV of water and 3BV of 30% ethanol aqueous solution to elute sugar and other impurities , and then eluted with 5BV65% ethanol aqueous solution, and the eluent was concentrated under reduced pressure to dryness to obtain the total triterpene extract. Reversed-phase preparation of high performance liquid phase for further separation and purification, using C-18 bonded silica gel as the stationary phase, acetonitrile-0.3% trifluoroacetic acid (30:70) solution as the mobile phase, the flow rate was set at 30ml / min, and UV detection was set The wave length of the instrument is 210nm, and the fractions of rosinic acid and palindromic acid are collected in sections, and the reagent is recovered to a small volume, placed for crystallization, and the crystallization is fi...

Embodiment 2

[0027] Take 1Kg of Gugongguo medicinal material, pulverize it, add 5L of 70% ethanol for ultrasonic extraction three times, combine the extracts, concentrate to low alcohol, absorb on macroporous resin, first use 2BV of water and 3BV of 30% methanol aqueous solution to elute sugar and other impurities, then Use 5BV70% methanol aqueous solution for elution, and the eluate is concentrated under reduced pressure to dryness to obtain the total triterpene extract. The obtained total triterpene is dissolved in a small amount of methanol, diluted with mobile phase, filtered through a 0.22 μm filter membrane, and then reversed-phase Prepare high performance liquid phase for further separation and purification, use C-18 bonded silica gel as the stationary phase, acetonitrile-0.3% trifluoroacetic acid (32:68) solution as the mobile phase, set the flow rate to 30ml / min, and set the wavelength of the UV detector 210nm, collect the rosic acid fraction and the potentinic acid fraction in sec...

Embodiment 3

[0029] Take 5Kg of Gugongguo medicinal material, crush it, add 40L50% ethanol to ultrasonically extract twice, combine the extracts, concentrate to low alcohol, and adsorb on macroporous resin, first use 2BV water and 3BV25% propanol aqueous solution to elute sugar and other impurities, Then eluted with 5BV70% propanol aqueous solution, and the eluate was concentrated under reduced pressure to dryness to obtain the total triterpene extract. The total triterpene was dissolved in a small amount of methanol, diluted with mobile phase, filtered through a 0.22 μm filter membrane, and then used Reversed-phase preparation of high performance liquid phase for further separation and purification, with C-18 bonded silica gel as the stationary phase, acetonitrile-0.3% trifluoroacetic acid (35:65) solution as the mobile phase, the flow rate was set at 30ml / min, and UV detection was set The wave length of the instrument is 210nm, and the fractions of rosinic acid and palindromic acid are co...

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PUM

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Abstract

The invention belongs to the field of separation of natural products, and provides a joint preparation method for euscaphic acid and tormentic acid. The preparation method comprises the following steps of: extracting with an ethanol liquid; treating with macroporous resin; eluting sugars and other impurities with water and a low-concentration aqueous solution serving as a water-soluble organic solvent; eluting with a high-concentration aqueous solution serving as a water-soluble organic solvent; concentrating the eluent under reduced pressure to dryness to obtain a total triterpene extract; purifying with an efficient liquid phase preparative chromatograph; segmentally collecting an euscaphic acid fraction and a tormentic acid fraction; and thermally refluxing and crystallizing with methanol to obtain high-purity euscaphic acid and tormentic acid. A product prepared with the method has high product purity and good quality.

Description

technical field [0001] The invention belongs to the field of separation of natural products, and in particular relates to a method for simultaneously preparing rosic acid and pollentinic acid from Gungung fruit by using high-performance liquid phase preparative chromatography. Background technique [0002] Gu Gong Guo Rosa odorata Sweet var. gigantea Rehd.et Wils. belongs to the Rosa plant. Its roots are flat and sour, and it has the effect of astringent intestines and antidiarrheal. It is often used to treat diarrhea, bacillary dysentery and other diseases. It is a folk medicinal material of the Yi nationality with a long history of blind use. Modern studies have shown that the root of G. quinquefolius contains a variety of triterpenoids, which have good analgesic and anti-inflammatory effects, and rosic acid and bilingic acid are the triterpenoids with relatively high amounts. In addition, studies by Liu Liang et al. have shown that the triterpenoids of Potentilla trifol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
Inventor 刘东锋吴艳波
Owner NANJING ZELANG MEDICAL TECH
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