A kind of preparation method of high-purity gentiopicroside

Abstract

The invention discloses a preparation method of high-purity gentiopicroside, which comprises the steps of extracting gentian plants in a solvent, enriching them by macroporous resin chromatography, and purifying the material liquid through alumina or acid alumina. Refining, the purified liquid is concentrated to recover the alcohol, the extract is dried, the methanol is crystallized, the crystal is precipitated by centrifugation, and dried to obtain gentiopicroside with a purity of more than 90%, then recrystallized, and the crystallization is dried to obtain a gentian with a purity of more than 98%. picroside monomer. The solvent and the separation medium involved in the invention can be reused, have good reproducibility, simple operation, and are suitable for industrial mass production.

Description

technical field [0001] The invention relates to the technical field of extraction and separation of split iridoid glycosides, in particular to a preparation method of high-purity gentiopicroside. Background technique [0002] Gentiopicroside is a cleavage iridoid glycoside compound, containing sugar group, high polarity, hygroscopic and unstable under acid, alkali, strong light and high temperature conditions. It is the main functional component of traditional Chinese herbal medicines such as gentian, chinensis, swedia, etc. and Chinese patent medicines. and other effects. The main functions of gentiopicroside in cosmetics are anti-allergy, redness and swelling, itching, inhibition of atopic dermatitis and allergies, and anti-inflammatory effect; in addition, it also has the effect of clearing away heat and dampness, which can improve dry skin. Sensitive and uncomfortable states such as itching, itching, etc., enhance the natural immunity of the skin; the activation of gen...

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%.