Method for preparing paeoniflorin and albiflorin

A technology of paeoniflorin and alba paeoniflorin, which is applied in the field of preparation of paeoniflorin and alba peony, can solve the problems that paeoniflorin and alba paeoniflorin cannot be separated, the operation of column packing and detection is complicated, and it is difficult to realize industrial production. Effects of recovery and recycling, realization of automation and operability, and simplification of process burden

Active Publication Date: 2012-06-13
SHANGHAI HUIWEN BIO TECH
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AI Technical Summary

Problems solved by technology

[0004] Through long-term research, the process of purifying total glucosides of paeoniflorin with macroporous resin technology is relatively mature, but paeoniflorin and paeoniflorin cannot be separated, and it is difficult to achieve the separation effect by general solvent extraction and other techniques
It is reported in the literature that paeoniflorin and paeoniflorin monomers are separated and purified by normal pressure silica gel column chromatography and high-speed countercurrent chromatography, but the former has low column efficiency, complicated column packing and detection operations, and the latter requires special equipment. It is difficult to achieve industrial production
At present, there are no commercially available products of paeoniflorin and paeoniflorin monomers on a large scale. Exploring a feasible industrial production process is a technical problem to be solved at present.

Method used

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  • Method for preparing paeoniflorin and albiflorin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1 macroporous resin static adsorption performance investigation

[0017] Weigh 1kg Radix Paeoniae Alba decoction pieces, extract twice with 8L of 70% ethanol under reflux, each time for 2h, filter, combine the filtrates, concentrate under reduced pressure until there is no alcohol smell, adjust the medicinal solution so that each 1ml medicinal solution is equivalent to 0.5g crude drug, and set aside.

[0018] Weigh 1.00g of the dry weight of each type of resin, place them in ten 50ml conical flasks with stoppers, add 10ml of Radix Paeoniae Alba extract (0.5g crude drug / ml), shake in a constant temperature shaking box at 35°C for 6h, The vibrating speed was 180prm, and the adsorbed Radix Paeoniae Alba extract was vacuum filtered, and the filtrate was properly diluted, and the contents of Paeony Radix and Radix Paeoniae Alba were determined by HPLC with reference to the method of the 2010 edition of Pharmacopoeia. The adsorbed resin was washed with water for 3 ...

Embodiment 2

[0025] The preparation of embodiment 2 Radix Paeoniae Alba extract

[0026] Weigh 40kg of Radix Paeoniae Alba, soak overnight in 70% ethanol, reflux extraction twice, each time for 2 hours, filter, combine the filtrate, and rotary evaporate until there is no alcohol smell, adjust the liquid so that every 1ml of liquid is equivalent to 0.5g of crude drug, spare. Weigh 120kg (wet weight) of LX38 resin, put it into a stainless steel column (300×2300cm), the column volume is 60L, load the sample, after adsorption for 1h, first remove impurities with 300L of water, 300L of 10% ethanol, and then use 360L of 50% ethanol Elute paeoniflorin and paeoniflorin, and finally regenerate the resin with 95% ethanol at a flow rate of 150-200L / h. Concentrate and evaporate the 50% ethanol part to obtain 2.52kg, wherein the purity of paeoniflorin is 24%, and that of paeoniflorin is 16 %.

Embodiment 3

[0027] The preparation of embodiment 3 Radix Paeoniae Alba extract

[0028] Weigh 40kg Radix Paeoniae Alba decoction pieces, soak overnight with 70% ethanol, reflux extraction twice, each time for 2 hours, filter, combine the filtrate, rotary evaporate to no alcohol smell, adjust the liquid medicine so that every 1ml liquid medicine is equivalent to 0.5g crude drug, spare. Weigh 120kg (wet weight) AB-8 resin, put it into a stainless steel column (300×2300cm), the column volume is 60L, load the sample, after adsorption for 1h, first remove impurities with 300L of water and 300L of 10% ethanol, and then use 50% Elute paeoniflorin and paeoniflorin with 360L of ethanol, and finally regenerate the resin with 95% ethanol at a flow rate of 150-200L / h. Concentrate and evaporate the 50% ethanol part to obtain 2.32kg, wherein the purity of paeoniflorin is 22%, and the purity of paeoniflorin is 22%. 12%.

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Abstract

The invention discloses a method for preparing paeoniflorin and albiflorin, which mainly includes the following steps: selecting peony plant raw materials containing the paeoniflorin and the albiflorin, adopting water or alcohol-water mixed solvent to perform extraction, mixing extract, concentrating, filtering, absorbing the obtained crude extract by adopting pre-preprocessed macroporous resin, performing gradient elution by using ethanol-water mixed solvent, collecting 30% to 75% of ethanol elution parts eluent to perform concentration and drying. The obtained refined extract adopts pressurized column chromatography, using silica gel and modified silica gel as fillers, appropriate organic solvent is separated in mobile phase, flow parts containing the paeoniflorin and the albiflorin are collected respectively, concentrated and dried to obtain paeoniflorin finished products and albiflorin finished products with the purity more than 90%. The method for preparing the paeoniflorin and the albiflorin is concise in process, strong in operability, convenient in automation, capable of achieving comprehensive utilization of plant resources, convenient in solvent recycling, low in energy consumption, high in product purity, easy to achieve and high in industrialization.

Description

technical field [0001] The invention relates to a preparation method of paeoniflorin and paeonin. technical background [0002] Paeoniflorin (paeoniflorin) and albiflorin (also known as paeoniflorin, albiflorin) are a kind of monoterpene glycosides, which are commonly found in Paeoniaceae plants, and are the main ingredients in traditional Chinese medicines such as Paeoniae Alba, Radix Paeoniae Rubra, and Cortex Moutan. Active ingredients and quality control standards, with a variety of pharmacological effects and uses, total glucosides in white spoon is a kind of medicine for treating rheumatoid arthritis in China, paeoniflorin and paeoniflorin can be used as active ingredients in related medicines and functions food field. [0003] The research literature on the preparation process of total paeoniflorin is mainly concentrated in my country. You Song et al. (Chinese Patent Application No. 02133298.3) disclose a "composition of paeoniflorin and paeonifloride and its prepar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08
Inventor 刘江云王蓉彭晓国冯育林杨世林
Owner SHANGHAI HUIWEN BIO TECH
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