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Process for preparing erythricine from gentian

A technology of gentianine and gentianogen, which is applied in the field of preparation technology of gentianine in gentian, can solve the problems of low yield, large loss and pollution, complicated process, etc.

Inactive Publication Date: 2011-01-12
刘树民
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] About the preparation method of gentianine, there are literature reports in China, adopt gentiopicroside to convert into gentianine through alkaline treatment, and then obtain the product through repeated column chromatography on a silica gel column, such as Northwest University master's degree thesis "Monoterpene indole Biomimetic Synthesis of Gentiana Decoction of Pyridine Alkaloids "Compound Research on Gentianine Decoction" mentions that gentiopicroside is converted by ammonia water with gentianine, and less gentianine (10g gentiopicrin) obtained by repeated silica gel column chromatography Only 0.07g of picroside was obtained). In addition, it was also obtained by rough extraction of alkalized Gentiana and then obtained by silica gel column chromatography. Obtain gentianin, but its technique is more complicated (gentiopicroside needs to be obtained earlier in the extraction process), and the output is not high, and a large amount of organic solvents are used (mostly using chloroform and methanol as solvents in the chromatography process, repeatedly Larger loss and pollution during chromatography). At the same time, silica gel for chromatography is a renewable material, which is not conducive to industrial production), which limits the application field of the process

Method used

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Examples

Experimental program
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Effect test

example 1

[0013] Take by weighing 500g gentian medicinal material, crush through a 20-mesh sieve, soak the liquid with a hydrophilic alkaline organic solvent at 8:1, pH=8-10, reflux extraction twice the next day, and the extraction temperature is 2 hours each time. Combine the extracts at 50°C, and recover the solvent under reduced pressure. The recovered solvent is monitored with a density agent and a pH reagent, and the recovered solution is adjusted to be the same as the original extract, so that it can be used repeatedly. Double the amount of extract, dissolve in water, extract 4 times with dichloromethane 2:1, recover the dichloromethane layer under reduced pressure, add 1 times the amount of acid water to dissolve, let it stand for 24 hours, filter to remove the precipitate, the filtrate is filtered through strong acid cation exchange resin, and the column The inner diameter is 2.5cm, the height is 22cm, washed with distilled water until colorless, then washed with 40% ethanol unti...

example 2

[0015] Weigh 1000g gentian medicinal material, pulverize through a 20-mesh sieve, soak the liquid with a hydrophilic alkaline organic solvent at 10:1, pH=8-10, reflux extraction 3 times the next day, and the extraction temperature is 3 hours each time. Combine the extracts at 55°C, recover the solvent under reduced pressure, monitor the recovered solvent with a density agent and pH reagent, adjust the recovered solution to be the same as the original extract, so that it can be used repeatedly. Double the amount of extract, dissolve in water, extract 5 times with chloroform 2:1, recover the dichloromethane layer under reduced pressure, add 2 times the amount of acid water to dissolve, let it stand for 24 hours, filter to remove the precipitate, and the filtrate is passed through strong acid type cation exchange resin, column The inner diameter is 5.5cm, the height is 45cm, washed with distilled water until colorless, and then washed with 50% ethanol until colorless, then eluted ...

example 3

[0017] Take by weighing 1500g gentian medicinal material, pulverize and cross 20 mesh sieves, soak the liquid with a hydrophilic alkaline organic solvent at 12:1, pH=8-10, reflux extraction 4 times the next day, each 2 hours extraction temperature is Combine the extracts at 60°C, and recover the solvent under reduced pressure. The recovered solvent is monitored with a density agent and a pH reagent, and the recovered solution is adjusted to be the same as the original extract, so that it can be used repeatedly. The extract was dissolved in double the amount of water, extracted 3 times with chloroform 4:1, and the chloroform layer was recovered under reduced pressure, then added 5 times the amount of acid water to dissolve, left for 24 hours, filtered to remove the precipitate, the filtrate was filtered through a strong acid cation exchange resin, and the column The inner diameter is 6.5cm, the height is 60cm, washed with distilled water until colorless, then washed with 40% eth...

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Abstract

The invention relates to a process for extracting erythricine from a gentianaceae plant acting as a gentian source, which comprises the following steps: making rhizome powder of raw gentian medicinal materials into coarse powder, carrying out reflux extraction in the environment of alkaline water bath of 60-100 DEG C for 2-4 hours with a hydrophilic organic solvent of which the amount is 2-20 times more than that of the coarse powder, carrying out vacuum filtration while hot, recovering the filtrate while depressurizing, processing the obtained solvent and reusing the processed solvent, and drying the extract while depressurizing to obtain a crude erythricine product 3; dissolving the crude erythricine product in a hydrophilic solvent, extracting with a lipophilic organic solvent according to a ratio of 2-4:1, recovering the hydrophilic organic solvent layer while depressurizing, and drying to obtain a crude erythricine product 2; and dissolving the crude erythricine product 2 in an acidic water solution, filtering to obtain a solution, enriching the solution with a resin column, and carrying out chromatography with a chromatographic column to obtain a refined erythricine product. The invention has the characteristics of simple process, low cost, low pollution, high product yield and purity and the like.

Description

technical field [0001] The invention belongs to the field of medicine preparation technology, in particular to the preparation technology of gentianine in gentiana. Background technique [0002] Gentian is the dry root and rhizome of plants such as Gentiana Gentiana, Gentiana three-flowered Gentiana, Gentiana barbata or Gentiana genus in the Gentianaceae family. It is mainly distributed in Northeast China and North China. Its pharmacologically active ingredients are gentiopicroside, gentianine, and gentianalin, etc. At present, it is believed that gentianine is derived from the structural modification and transformation of gentiopicroside, the split iridoid glycosides represented by gentiopicroside in gentiana. Studies have shown that gentiopicroside can pass through intestinal The action of the intestinal flora is converted into gentianine, and the pharmacological action of gentian is the synergistic effect of gentiopicroside and gentianine. Pharmacological studies have s...

Claims

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Application Information

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IPC IPC(8): C07D491/052
Inventor 刘树民刘学伟
Owner 刘树民
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