Process for preparing erythricine from gentian

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...

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