Method for synchronized preparation of pinocembrin and 2', 4'-dihydroxy chalcone from oxytropis falcate bunge

A technology of hydroxychalcone and Oxytropis falciparum, which is applied in the field of extracting flavonoid active substances, can solve the problems of complex composition of column chromatography elution solvent system, difficulty in large-scale production, cumbersome steps, etc., and save production raw materials , avoid the use of toxic reagents, the effect of simple process

Active Publication Date: 2013-04-24
GANSU CHEEZHENG TIBETAN MEDICINE CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The methods for preparing flavonoid monomers are mostly laboratory methods, with cumbersome steps and low preparation volume, mostly milligram-level
Chinese patent application No. 200910264515.1 provides a method for preparing flavone monomer 2',4'-dihydroxychalcone, but this method requires the use of dichloromethane as a toxic reagent, and the composition of the column chromatography elution solvent system is complicated. It is also necessary to use special equipment for high-performance liquid chromatography for purification, and the preparation amount is low, so it is difficult to achieve large-scale production

Method used

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  • Method for synchronized preparation of pinocembrin and 2', 4'-dihydroxy chalcone from oxytropis falcate bunge

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] [Example 1] Simultaneous preparation of pinocin and 2',4'-dihydroxychalcone from Oxytropis falciparum

[0020] Take 6 kg of Oxytropis falciparum, grind it, and extract it 3 times with 48L of 90% ethanol under reflux, filter each extract, and concentrate the filtrate under reduced pressure to obtain a total extract of 720 g. Suspend the total extract in 2000mL of water, extract twice with 1000mL of petroleum ether and 6 times with 1000mL of ethyl acetate, combine the ethyl acetate extracts, and recover the solvent under reduced pressure to obtain 200g of ethyl acetate extract. Take the ethyl acetate extract, mix the sample with 200g 200-300 mesh silica gel, evaporate the solvent, and take another 1700g 200-300 mesh silica gel, and put it on a common glass chromatography column with petroleum ether-ethyl acetate wet method with a volume ratio of 20:1. Add the sample, first elute with 18L (4 times column volume) of petroleum ether-ethyl acetate at a volume ratio of 20:1, d...

Embodiment 2

[0021] [Example 2] Simultaneous preparation of pinocin and 2',4'-dihydroxychalcone from Oxytropis falciparum

[0022] Take 1 kg of Oxytropis falciparum, crush it, and extract 3 times with 10L of 90% ethanol under reflux, filter each extract, and concentrate the filtrate under reduced pressure to obtain 125 g of total extract. Suspend the total extract in 500 mL of water, extract 3 times with 500 mL of petroleum ether, and 7 times with 500 mL of ethyl acetate, combine the ethyl acetate extracts, recover the solvent under reduced pressure, and obtain 35 g of ethyl acetate extract. Take the ethyl acetate extract, mix the sample with 35g of 200-300 mesh silica gel, evaporate the solvent to dryness, and take another 350g of 200-300 mesh silica gel, and put it on an ordinary glass chromatography column with a volume ratio of 20:1 petroleum ether-ethyl acetate wet method, Add the sample, first elute with 4.8L (5 times column volume) of petroleum ether-ethyl acetate with a volume rati...

Embodiment 3

[0023] [Example 3] Simultaneous preparation of pinocin and 2',4'-dihydroxychalcone from Oxytropis falciparum

[0024] Take 1 kg of Oxytropis falciparum, grind it, and extract it 4 times with 6L 95% ethanol under reflux, filter each extract, and concentrate the filtrate under reduced pressure to obtain 123 g of total extract. Suspend the total extract in 250 mL of water, extract twice with 500 mL of petroleum ether, and 6 times with 500 mL of ethyl acetate, combine the ethyl acetate extracts, recover the solvent under reduced pressure, and obtain 33 g of ethyl acetate extract. Take the ethyl acetate extract, mix the sample with 33g of 200-300 mesh silica gel, evaporate the solvent to dryness, and take another 200g of 200-300 mesh silica gel, and put it on an ordinary glass chromatography column with a volume ratio of 20:1 petroleum ether-ethyl acetate wet method, Add the sample, first use 3.3L (6 times column volume) to elute with petroleum ether-ethyl acetate at a volume ratio...

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Abstract

The present invention provides a method for synchronized preparation of pinocembrin and 2', 4'-dihydroxy chalcone from oxytropis falcate bunge. By using Tibetan herb oxytropis falcate bunge as a raw material, via steps such as heating extraction by ethanol, extraction by ethyl acetate, precipitation by petroleum ether, ordinary silica and reverse phase silica gel column chromatography, highly purified pinocembrin and 2 ', 4'-dihydroxy chalcone are obtained. The pinocembrin and 2', 4'-dihydroxy chalcone prepared by the method of the present invention both have purities greater than 98%, and both have relatively high yields and extraction rates, wherein the yield and extraction rates of the pinocembrin are respectively 0.08 % and 67.5%, and the yield and extraction rates of the 2 ', 4'-dihydroxy chalcone are respectively up to 0.24% and 88.9%.

Description

technical field [0001] The invention relates to the technical field of traditional Chinese medicine, in particular to a method for extracting flavonoid active substances from Oxytropis falciparum. Background technique [0002] Oxytropis falcata Bunge (Oxytropis falcata Bunge) is a perennial stemless herb of the genus Oxytropis of the Fabaceae family. It is widely distributed in Tibet, Qinghai, and southern Gansu. , western Sichuan and Xinjiang and other places. It has anti-inflammatory and pain-relieving, heat-clearing, detoxifying, and hemostatic effects. It can be used internally to treat influenza, tonsillitis, high fever, laryngitis, bronchitis, bleeding, constipation, anthrax, and yellow water disease in Tibetan medicine. External application can treat boils, swelling, pain, and trauma. , Bone pain. Because of its outstanding anti-inflammatory effect, it is the "three major anti-inflammatory drugs" of Tibetan medicine and enjoys the reputation of "king of herbs". It ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/32C07D311/40C07C49/835C07C45/78
Inventor 师彦平陈娟李波
Owner GANSU CHEEZHENG TIBETAN MEDICINE CO LTD
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