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Method for quickly extracting mussaenoside

A technology of methyl crocurinate and extraction method, which is applied in the fields of steroidal compounds and organic chemistry, and can solve the problems of difficult separation, high synthesis cost, and complex chemical synthesis, etc.

Inactive Publication Date: 2017-08-18
GUANGDONG PHARMA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But at present the chemical synthesis of aureidic acid methyl ester is more complicated, and the synthetic cost is higher; quite difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1. Mix the dry powder of 1000g Jade Yejin Flower with 10g calcium carbonate and put it into the extractor. Add 20 times the amount of 70% ethanol according to the mass-volume ratio (w / v, g / mL), heat at reflux at 80°C for 1 hour, and repeat the extraction twice. Combine the solutions, recover ethanol, and concentrate until there is no alcohol smell.

[0019] 2. The concentrated solution was first fully eluted with petroleum ether, and the aqueous layer was extracted three times with an equal amount of n-butanol. Mix the n-butanol liquids extracted three times, add lead acetate, and after standing still, filter with suction, recover n-butanol from the filtrate to obtain a concentrated solution.

[0020] 3. Take the silica gel and dry-pack the column, and first elute with a mixture of petroleum ether and ethyl acetate with a volume ratio of 1:2. Then, it is eluted with a mixture b composed of petroleum ether, ethyl acetate and methanol, and the volume ratio of each compo...

Embodiment 2

[0024] 1. Take 1000g of dry powder of Jade Yejinhua and mix with 10g of calcium carbonate and put it into the extractor. Add 20 times the amount of 85% ethanol according to the mass-volume ratio (w / v, g / mL), heat at reflux for 1 hour at 75°C, and repeat the extraction twice. Combine the solutions, recover ethanol, and concentrate until there is no alcohol smell.

[0025] 2. The concentrated solution was fully eluted with petroleum ether first, and the aqueous layer was extracted three times with an equal volume of n-butanol. Mix the n-butanol liquids extracted three times, add lead acetate, and after standing still, take the upper layer, recover n-butanol, and obtain a concentrated solution.

[0026] 3. Silica gel dry packing, first elute with a mixture of petroleum ether and ethyl acetate with a volume ratio of 2:1. Then, it is eluted with a mixture b composed of petroleum ether, ethyl acetate and methanol, and the volume ratio of each component in the eluent b is petroleum...

Embodiment 3

[0029] 1. Take 1000g of dry powder of Jade Yejinhua and mix with 10g of calcium carbonate and put it into the extractor. Add 25 times the amount of 70% ethanol according to the mass volume ratio (w / v, g / mL), heat at reflux at 70°C for 1 hour, and repeat the extraction twice. Combine the solutions, recover ethanol, and concentrate until there is no alcohol smell.

[0030] 2. The concentrated solution was fully eluted with petroleum ether first, and the aqueous layer was extracted three times with an equal volume of n-butanol. Mix the n-butanol liquids extracted three times, add lead acetate, and after standing still, take the upper layer, recover n-butanol, and obtain a concentrated solution.

[0031] 3. Silica gel dry packing, first elute with a mixture of petroleum ether and ethyl acetate with a volume ratio of 2:1. Then, it is eluted with a mixture b composed of petroleum ether, ethyl acetate and methanol, and the volume ratio of each component in the eluent b is petroleum...

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PUM

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Abstract

The invention discloses a method for quickly extracting mussaenoside. The method comprises the following steps of (1) uniformly mixing the mussaenda pubescens ait.f. and calcium carbonate, adding into an extracting device, heating and refluxing for 1 to 1.5h by ethanol, concentrating and filtering; (2) fully eluting the concentrated liquid by petroleum ether, extracting a water layer by n-butyl alcohol, adding lead acetate until the lead acetate is separated out, standing and precipitating, and obtaining supernatant; (3) feeding a sample by a dry type, and filtering by a silica gel column; firstly, using an eluting liquid A to elute, then using an eluting liquid B to elute, mixing the eluting liquid containing a target matter, concentrating, evaporating and drying, so as to obtain crude crystal; (4) dissolving the crude crystal by a small amount of hot ethyl acetate, recrystallizing at low temperature, and drying. The method has the advantages that by adopting the extracting scheme, the mussaenoside can be quickly extracted, and the method is suitable for the large-scale industrialized production of the mussaenoside; the purity of the mussaenoside reaches 95% or above by adopting the method.

Description

technical field [0001] The invention relates to the purification of compounds, in particular to a method for rapidly extracting japonica aureronate methyl ester. Background technique [0002] Yuyejinhua is mainly produced in Lingnan area, the original plant is Rubiaceae Yuyejinhua plant Yuyejinhua Mussaenda pubescens Ait. f. , has the effects of clearing heat and detoxifying, cooling blood and relieving summer heat, and is used for colds, heatstroke, fever, cough, enteritis, nephritis, edema, sore throat, bruises, snake bites, and poisoning of weed, cassava, and wild fungi. The ethyl acetate extraction part and the n-butanol extraction part of the water extract of Yuye Jinhua have a significant effect on inhibiting acute inflammation; among them, the iridoid component Yuye Jinhuacurinic acid methyl ester has been confirmed by pharmacological experiments to have obvious anti-inflammatory effects. , analgesic and antibacterial effects. But at present the chemical synthesi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J53/00
CPCC07J53/004
Inventor 孙继燕潘利明周中林
Owner GUANGDONG PHARMA UNIV
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