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Preparation method of high-purity paeoniflorin and albiflorin

The technology of paeoniflorin and paeoniflorin is applied in the field of preparation of high-purity paeoniflorin and paeoniflorin, and can solve the problems of poor separation of paeoniflorin and paeoniflorin, unsuitable repetition and amplification, large differences in column packing, and the like, To achieve the effect of long separation cycle, large preparation volume and increased production capacity

Active Publication Date: 2016-01-27
SHANGHAI TAUTO BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the process of purifying total glycosides of paeoniflorin using macroporous resin technology is relatively mature, but it is not easy to separate paeoniflorin and paeoniflorin, the column efficiency of silica gel column chromatography is low, and the difference in column packing is large, so it is not suitable for repetition and amplification. The content of glycosides is low, and the recovery rate is low by conventional column chromatography, which increases the production cost

Method used

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  • Preparation method of high-purity paeoniflorin and albiflorin
  • Preparation method of high-purity paeoniflorin and albiflorin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take the dried peony plant material and pulverize it, weigh 1000g, add 10L of 80% ethanol solution for ultrasonic extraction for 60 minutes each time, extract 3 times, and concentrate the extract under reduced pressure to obtain 200g of extract. Add 100 parts by mass of water to dissolve 1 part by mass of extract, extract with ethyl acetate, extract 3 times in total, combine the extracts to reclaim ethyl acetate to obtain 40g of extract, put the styrene macroporous resin column on the extract, and use a volume fraction of 25 % ethanol aqueous solution was used for elution, and the eluate was collected, concentrated and dried to obtain a crude extract, which was used for high-speed countercurrent separation.

[0026] Prepare a two-phase solvent system of carbon trichloride, n-butanol, methanol, and water in a separatory funnel, mix it at a volume ratio of 4:2:1:1, shake it, let it stand for stratification, and ultrasonically degas it for 30 minutes. Take the upper phase ...

Embodiment 2

[0028] Take the dried peony plant material and pulverize it, weigh 1000g, add 10L of 60% ethanol solution for ultrasonic extraction for 60 minutes each time, extract 3 times, and concentrate the extract under reduced pressure to obtain 200g of extract. Add 100 parts by mass of water to dissolve 1 part by mass of extract, extract with ethyl acetate, extract 3 times altogether, combine the extracts to reclaim ethyl acetate to obtain 40g of extract, put the styrene-based AB-8 macroporous resin column on the extract, and use Elute with 25% ethanol aqueous solution, collect the eluate, concentrate and dry to obtain a crude extract, which is used for high-speed countercurrent separation.

[0029] Prepare a two-phase solvent system of carbon trichloride, n-butanol, methanol, and water in a separatory funnel, mix it at a volume ratio of 4:1:3:2, shake it, let it stand for stratification, and ultrasonically degas it for 30 minutes. Take the upper phase and fill the high-speed countercu...

Embodiment 3

[0031] The dried peony plant material was crushed, weighed 1000g, added 10L of 70% ethanol solution for ultrasonic extraction for 60 minutes each time, extracted 3 times, and the extract was concentrated under reduced pressure to obtain 300g of extract. Add 100 parts by mass of water to dissolve 1 part by mass of extract, extract with ethyl acetate, extract 3 times altogether, combine the extracts to reclaim ethyl acetate to obtain 50g of extract, put the styrene-based AB-8 macroporous resin column on the extract, and use Elute with 50% ethanol aqueous solution, collect the eluate, concentrate and dry to obtain a crude extract, which is used for high-speed countercurrent separation.

[0032]Prepare a two-phase solvent system of carbon trichloride, isobutanol, methanol, and water in a separatory funnel, mix at a volume ratio of 4:2:2:1, shake, let stand for stratification, and ultrasonically degas for 30 minutes. Take the upper phase and fill the high-speed countercurrent chrom...

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Abstract

The invention relates to a preparation method of high-purity paeoniflorin and albiflorin. The method includes the steps of firstly, adding smashed paeoniaceae plant raw materials containing paeoniflorin and albiflorin to an ethanol solution, conducting ultrasonic extraction, concentrating an extracting solution to obtain extract, dissolving extract with water, and conducting extraction and pressure reduction concentration to obtain extract; secondly, eluting extract with an alcohol-water solution through column chromatography with macroporous resin as filler, collecting flow components containing paeoniflorin and albiflorin, and conducting concentrating and drying to obtain coarse extract; thirdly, separating out the coarse extract through a high-speed countercurrent chromatography method, conducting online monitoring through an ultraviolet detector, collecting flow components and pressure reduction concentration, and conducting crystallizing and drying to obtain paeoniflorin and albiflorin, wherein a solvent system of the high-speed countercurrent chromatography is prepared from carbon trichloride, butyl alcohol, methyl alcohol and water. Paeoniflorin and albiflorin prepared through the method are high in product purity and good in quality, are suitable for high-speed countercurrent chromatographs of various types and can be easily and industrially amplified.

Description

technical field [0001] The invention belongs to the field of extraction and separation of natural medicines, in particular to a preparation method of high-purity paeoniflorin and paeoniflorin. Background technique [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 related to the preparation process of paeoniflorin and paeoniflorin is mainly concentrated as follows: You Song et al. (Chine...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08
Inventor 王维娜邓力
Owner SHANGHAI TAUTO BIOTECH CO LTD
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