Preparation method of high-purity gentiopicroside

Abstract

The invention discloses a preparation method of high-purity gentiopicroside, which comprises the following steps of: extracting a gentian plant in a solvent, enriching by macroporous resin chromatography, refining the purified feed liquid by aluminum oxide or acidic aluminum oxide, concentrating the refined liquid to recover alcohol, drying extract, crystallizing by methanol, centrifugally separating crystal precipitate, and drying to obtain the high-purity gentiopicroside. The gentiopicroside with the purity larger than 90% is obtained, then recrystallization is conducted, crystals are dried, and the gentiopicroside monomer with the purity larger than 98% is obtained. The solvent and the separation medium involved in the method can be recycled, and the method is good in reproducibility, simple to operate and suitable for industrial batch production.

Description

technical field [0001] The invention relates to the technical field of extraction and separation of secoiridoid glycosides, in particular to a preparation method of high-purity gentiopicroside. Background technique [0002] Gentiopicroside belongs to secoiridoid glycoside compounds, containing sugar groups, high polarity, hygroscopicity and instability under acid, alkali, strong light and high temperature conditions. It is the main functional ingredient of traditional Chinese medicinal materials Gentiana, Gentiana, Swertia, etc. and Chinese patent medicines. It has a variety of physiological activities, such as gallbladder, liver protection, stomach invigoration, blood pressure reduction, anti-inflammatory, anti-oxidation, antibacterial and other effects. The main effects of gentiopicroside in cosmetics are anti-allergic, redness-reducing, and itching-relieving, and it can inhibit irritation and anti-inflammatory effects on atopic dermatitis and allergies; it also has the e...

AI Technical Summary

Problems solved by technology

[0003] At present, the preparation process of high-purity gentiopicroside has been reported in the literature, such as using different resins for multiple purifications to improve the purity. This technology has the problems of large reagent usage, long production cycle and relatively high cost.

Wherein, the technique of ion exchange resin purification is used, and a large amount of acid or alkali solution needs to be used when the ion exchange resin is regenerated, which has safety and environmental protection problems; in addition, the extract (gentiopicroside ≥ 50%) of macroporous resin purification The pH value of the aqueous solution (when the concentration of the extract is 2500mg / L) is 3 to 4, which is weakly acidic. Add dilute lye to adjust the pH to 8.0. The concentration of gentiopicroside in the aqueous solution is detected by HPLC, which is reduced from the initial value of 1250mg / L to 1106mg / L. L, indicating that gentiopicroside is unstable, so the use of weak base and basic anion exchange resin to purify gentiopicroside will degrade it, resulting in low yield, and the content of gentiopicroside in the purified extract may not improve significantly

Use weakly acidic or acidic cation exchange resin for purification, because the aqueous solution of gentian extract is acidic, it is difficult for the acidic substance to undergo ion exchange with the resin, and finally the purity of gentiopicroside does not increase significantly

And directly use reverse phase liquid phase to prepare high-purity gentiopicroside, its equipment and filler are expensive, and large-scale production is not as efficient and cheap as the present invention

Another example is the use of cheap silica gel for column chromatography purification of the feed solution after resin purification, which is inefficient and requires a large amount of organic reagents during desorption. Generally, two or more reagents of different polarities are required to be used in combination, and silica gel high regeneration cost

Up to now, there is no fast, efficient, mass-produced, high-yield and cheap preparation process for gentiopicroside with a purity of 90% or more than 98%.