Preparation method of high-purity gentiopicroside

A gentiopicroside, high-purity technology, applied in the field of preparation of high-purity gentiopicroside, can solve the problems of insufficient scale production, low yield, low efficiency, etc., to avoid solvent residues, wide range of raw materials, solvent Operational Security Effects

Active Publication Date: 2021-08-13
劲牌持正堂药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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 ...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Use a crusher to crush the dried gentian medicinal materials into small pieces with a length less than 1cm, put them into an extraction tank, add water 15 times that of the dry material, extract 2.0 hours at a temperature of 80°C, and then filter, repeat the above process, and then extract Twice, combine the filtrates, and adsorb the filtrates on the pretreated D101 resin column at a flow rate of less than 1BV / h. The amount of resin used is twice the amount of extracted and input medicinal materials, and the ratio of diameter to height of the resin column is 1:8. After the feeding and adsorption of feed liquid, use 4BV water to elute and remove impurities at the flow rate of feeding liquid sample, then use 5BV volume fraction of 10% ethanol aqueous solution to elute, analyze and adsorb at a flow rate of 1BV / h, and collect the eluate . Then the eluate is refined with a neutral alumina column, the amount of neutral alumina is 0.05 times the amount of medicinal materials f...

Embodiment 2

[0027] Use a crusher to crush the dried gentian medicinal material into small pieces with a length less than 3 cm, put it into an extraction tank, add 70% ethanol 10 times that of the dry material, extract 2.0 hours at 80°C, and then filter, repeat the above process, Extract again 2 times, combine the filtrate, concentrate the filtrate to the alcohol content of the concentrate lower than 10%, add an appropriate amount of water and mix evenly, so that the final volume of the feed liquid is about 15 times (v / g) of the amount of medicinal material that is extracted and put into it, and then The material liquid is adsorbed on the pretreated AB-8 resin column at a flow rate of less than 1BV / h. The amount of resin used is 3 times the amount of extracted and input medicinal materials, and the ratio of diameter to height of the resin column is 1:10. After the sample loading and adsorption of feed liquid, use 5BV water to elute and remove impurities at the flow rate of feed liquid sampl...

Embodiment 3

[0029]Use a crusher to crush the dried gentian medicinal material into small pieces with a length less than 5 cm, put it into an extraction tank, add 12 times the amount of the dry material to a 30% methyl ethanol aqueous solution, and extract it in circulation at a water temperature of 80°C for 1.5 hours, and then filter. Repeat the above process, extract 2 more times, combine the filtrates, concentrate until there is no alcohol smell, reclaim methanol, and then add an appropriate amount of water to the concentrated solution, so that the total volume of the feed solution is about 20 times the amount of medicinal materials that are extracted (v / g ), mix evenly, and then adsorb the feed liquid on a pretreated D101 resin column at a flow rate of less than 1BV / h. The amount of resin is 2.5 times the amount of extracted medicinal materials, and the ratio of diameter to height of the resin column is 1:12. After the sample loading and adsorption of feed liquid, use 5BV water to elute...

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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...

Claims

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Application Information

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IPC IPC(8): C07H17/04C07H1/08
CPCC07H17/04C07H1/08
Inventor 吕庆银陈志元王玉张继斌孙代华李名洁
Owner 劲牌持正堂药业有限公司
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