Method for extracting high-purity loganin from cornus officinalis fruits

A technology of cornus officinalis and loganin, which is applied in the field of purifying loganin, can solve the problems of being difficult to meet industrialized large-scale production, being unsuitable for industrial-scale production, and using a large amount of solvents, and achieves fewer types of solvents, easy operation, and improved performance. Effects of yield and purity

Active Publication Date: 2017-05-10
LUNAN PHARMA GROUP CORPORATION
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  • Application Information

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Problems solved by technology

Chinese invention patent "Method for preparing loganin from traditional Chinese medicine Cornus officinalis", application number 201310415843.3, mainly prepares loganin through ethanol heating extraction, macroporous resin adsorption, silica gel column chromatography, recrystallization and other steps. This patent uses silica gel column Chromatography, using mixed solvent gradient elution to purify loganin, the solvent us

Method used

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Embodiment 1

[0026] Take 1kg of dried fruit of Cornus officinalis, add 7L of ethanol with a volume fraction of 50%, heat and reflux to extract twice, each extraction for 1 hour, combine the two extracts, concentrate, add ethanol to adjust the alcohol concentration to 30%, add 1 / 20 volume 2mol / L acetic acid, react at 80°C for 2 hours, after the reaction is completed, add NaOH solution to neutralize to neutral, and concentrate the neutralized solution to dryness to obtain a dry product, which is extracted twice with 400mL ethanol under reflux, each time for 2 hours, The liquids were combined and concentrated to obtain crude loganin. The crude product was dissolved with 100 mL of methanol under reflux, and the insoluble matter was filtered while it was hot. The filtrate was cooled to room temperature, stirred and crystallized, filtered and dried, and recrystallized twice with methanol to obtain 3.8 g of loganin with a content of 96.3%.

Embodiment 2

[0028] Take 1kg of dried fruit of Cornus officinalis, add 10L of ethanol with a volume fraction of 20%, heat and reflux to extract twice, each extraction is 2 hours, combine the two extracts, concentrate, add ethanol to adjust the alcohol concentration to 5%, add 1 / 10 volume 1mol / L hydrochloric acid, react at 70°C for 3 hours, after the reaction is over, add NaHCO 3 The solution was neutralized to neutral, and the neutralized solution was concentrated to dryness to obtain a dried product, which was extracted twice with 600 mL of acetone under reflux for 2 hours each time, and the extracts were combined and concentrated to obtain a crude loganin. The crude product was dissolved in 200 mL of absolute ethanol by heating under reflux, and the insoluble matter was filtered while it was hot. The filtrate was cooled to room temperature, stirred and crystallized, filtered and dried, and recrystallized twice with absolute ethanol to obtain 3.2 g of loganin with a content of 98.1%. . ...

Embodiment 3

[0030] Take 4kg of dried fruit of Cornus officinalis, add 32L of ethanol with a volume fraction of 60%, heat and reflux to extract twice, each extraction is 2 hours, combine the two extracts, concentrate, add ethanol to adjust the alcohol concentration to 70%, add 1 / 100 volume 3mol / L hydrochloric acid, react at 60°C for 4 hours, after the reaction is completed, add NaHCO 3 The solution was neutralized to neutral, and the neutralized solution was concentrated to dryness to obtain a dry product, which was extracted twice with 1 L of methanol under reflux, each time for 2 hours, and the extracts were combined and concentrated to obtain a crude loganin. The crude product was dissolved with 800 mL of ethanol under reflux, and the insoluble matter was filtered while it was hot. The filtrate was cooled to room temperature, stirred and crystallized, filtered and dried, and recrystallized twice with ethanol to obtain 16.2 g of loganin with a content of 97.2%.

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Abstract

The invention relates to a method for extracting high-purity loganin from cornus officinalis fruits. The method includes: using traditional Chinese medicine cornus officinalis fruits as the raw material, and performing reflux extraction, acid-reaction impurity removing, organic-solvent purification, crystallization, recrystallization and the like to obtain the loganin with the purity being larger than 95%. The method has the advantages that acid reaction is used to remove impurities which affects the crystallization, and the method is simple in process, low in production cost and suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the field of traditional Chinese medicine extraction, in particular to a method for purifying loganin from cornus officinalis. Background technique [0002] Cornus officinalis is the mature and dried pulp of Cornus officinalis, a traditional rare medicinal material and commonly used precious Chinese medicine in my country. It has the functions of astringent, sweating, and liver and kidney. It is one of the components of Liuwei Dihuang Pills for metrorrhagia, internal heat and thirst. Iridoid glycosides are one of the main active components of Cornus officinalis. As the main component of iridoid glycosides in Cornus officinalis, loganin has the functions of lowering blood sugar, anti-platelet aggregation, immune regulation, anti-shock, anti-oxidation, and inhibiting preadipocytes. differentiation etc. At present, this component has become a hot spot in the research of Cornus officinalis, and has broad development prospects. ...

Claims

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Application Information

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IPC IPC(8): C07H1/08C07H17/04A61K31/7048A61P3/10A61P7/02A61P37/02A61P39/06
Inventor 张贵民马素燕梁红宝
Owner LUNAN PHARMA GROUP CORPORATION
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