Method for producing ginsenoside Rh4 by utilizing panaxatriol ginsenoside through large-scale conversion

A large-scale technology of ginsenoside, applied in chemical instruments and methods, organic chemistry, glycoside steroids, etc., can solve the problems of inability to realize large-scale production, strict operation requirements, complicated process, etc., to improve market competitiveness, refine and purify The effect of simple process and low production cost

Inactive Publication Date: 2016-10-26

NORTHWEST UNIV

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AI-Extracted Technical Summary

Problems solved by technology

However, ginsenosides are degraded in strong acid and strong alkali solutions to generate more by-products, and the components are very complex, which has a certain impact on the separation and purification of later compounds; the enzymatic degradation conver...

Abstract

The invention discloses a method for producing ginsenoside Rh4 by utilizing panaxatriol ginsenoside through large-scale conversion, belonging to the field of biochemical industry. The method comprises the following steps: dissolving the panaxatriol ginsenoside in deionized water in a fermentation tank, introducing N2 for protection, then carrying out online sterilization, adding an organic acid solution and a heteropoly acid HxYW12O40-nH2O catalyst with a Keggin structure and a certain catalytic amount, wherein Y is selected from the group consisting of P, Si, Fe or Zn, and x is 3 or 4 and n is a positive integer of 0 to 30, then carrying out a directional conversion reaction under the protection of N2 at a constant temperature and in a constant pressure, and finally collecting a reaction product and carrying out purifying so as to obtain high-purity ginsenoside Rh4, wherein the condition of online sterilization is at 121 DEG C for 20 min; N2 is introduced for protection before online sterilization; and added organic acid is a combination of one or more selected from the group consisting of lactic acid, malic acid, citric acid, alpha-ketoglutaric acid, succinic acid, trans-butenoic acid and pyruvic acid. The method provided by the invention has the advantages of simple and practicable process, fewer side reactions, high product purity and facilitation to industrial production.

Application Domain

Organic active ingredientsDispersion delivery +5

Technology Topic

Organic acidChemistry +13

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Examples

Experimental program(5)

Example Embodiment

[0019] Example 1

[0020] Add 65L of deionized water to a fully automatic fermenter with an effective volume of 100L, then add 3500g of ginsenoside Rg1 with a purity of 85% (impurities are other types of ginsenosides and polysaccharides), pass N 2 , the ventilation flow rate is 50 L/min, and lasts for 5 minutes, then stops the ventilation and starts the heating-in-line sterilization, and the sterilization condition is 121°C, and maintains for 20 minutes. After cooling down to below 90°C, add 5 L of sterile citric acid solution with a concentration of 0.15 mol/L and 10 g of heteropoly acid H 3 PW 12 o 40 ·5H 2 0, then heat the liquid in the fermenter to 90°C and keep it for 48h, while keeping the stirring speed at 200rpm, put all the liquid out of the container and let it stand for 12h after the reaction, collect the supernatant 20L and dry it to obtain the crude product of ginsenoside Rh4 about 3120g, the purity of ginsenoside Rh4 detected by HPLC is 92%.

Example Embodiment

[0022] Example 2

[0023] Add 300L of deionized water to a fully automatic fermenter with an effective volume of 500L, and then add 90kg of ginsenoside Rg2 with a purity of 95% (the impurities are other types of ginsenosides and polysaccharides), pass N 2 , the ventilation flow rate is 350 L/min, and lasts for 4 minutes, and then the ventilation is stopped to start the online sterilization, and the sterilization condition is 121°C, and it is maintained for 20 minutes. After cooling down to below 90°C, add 20L of sterile malic acid solution with a concentration of 0.8mol/L, 10L of sterile succinic acid solution with a concentration of 0.6mol/L and 20g of heteropoly acid H 4 SiW 12 o 40 25H 2 0, then heat the fermenter to 75°C and keep it for 36 hours while keeping the stirring speed at 100rpm. After the reaction, all the liquid is released and left in the container for 24 hours, centrifuged to obtain 100L of supernatant, and there is about 120L of solid-liquid mixture at the bottom. Add 120L of deionized water, stir the bottom mixture evenly, wash once, let it stand for 12 hours, centrifuge to get the supernatant, collect the liquid and dry it to obtain about 82kg of ginsenoside Rh4 crude product, and the purity of ginsenoside Rh4 detected by HPLC is 93%.

Example Embodiment

[0024] Example 3

[0025] Add 120L of deionized water to a fully automatic fermenter with an effective volume of 200L, then add 28kg of ginsenoside Rf with a purity of 90% (the impurities are other types of ginsenosides and polysaccharides), pass N 2 , the ventilation flow rate is 200 L/min, and lasts for 3 minutes, then stops the ventilation and starts the online sterilization, the sterilization condition is 121°C, and maintains for 20 minutes. After cooling down to below 90°C, add 10L of sterile malic acid solution with a concentration of 0.3mol/L, 10L of α-ketoglutaric acid solution with a concentration of 0.25mol/L, 225mL of lactic acid and 30g of heteropoly acid H 3 FeW 12 o 40 ·30H 2 O, then heat the fermenter to 90°C and keep it for 48 hours, while keeping the stirring speed at 300rpm. After the reaction is over, release all the liquid and let it stand in the container for 24 hours. Take 60L of the supernatant, and centrifuge about 40L of the liquid containing the precipitate at the remaining bottom. Add 40L of deionized water to wash the supernatant again, stir the bottom mixture evenly and then let it stand for 24h, centrifuge to get the supernatant, collect all the supernatant and dry to obtain about 24kg of ginsenoside Rh4 crude product, and HPLC detects ginsenoside Rh4 The purity is 92%.

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Classification and recommendation of technical efficacy words

Improve conversion rate
Improve catalytic effect

Method for producing ginsenoside Rh4 by utilizing panaxatriol ginsenoside through large-scale conversion

AI-Extracted Technical Summary

Problems solved by technology

Abstract

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Examples

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Example Embodiment

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Description & Claims & Application Information

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