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Method for preparation of loganin from traditional Chinese medicine Cornus officinalis

A technology of cornus officinalis and loganin, which is applied to the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of difficulty in large-scale production, low extraction efficiency, and low preparation volume, and achieve low cost, The effect of high extraction rate and high product content

Inactive Publication Date: 2015-03-25
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

) The method reported is ethanol immersion extraction, the extract is concentrated and centrifuged, the supernatant is separated by macroporous adsorption resin, the effluent is separated by normal phase silica gel column chromatography to obtain a white solid, and the white solid is separated by preparative high performance liquid chromatography. However, this method is soaked in ethanol, the extraction efficiency is low, and special equipment is required for preparative high-performance liquid chromatography, the preparation amount is low, and it is difficult to achieve large-scale production

Method used

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Examples

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Effect test

Embodiment 1

[0023] Take 50 g of the traditional Chinese medicine Cornus officinalis, crush it, pass through a 40-mesh sieve, heat and reflux with 400 mL of 65% ethanol to extract twice, filter each extract, combine, and concentrate under reduced pressure to obtain a total extract of 27.1 g. The total extract was dissolved by adding 25 mL of water, filtered, and the filtrate was applied to a macroporous adsorption resin column, firstly eluted with 1 times the column volume of water, discarded the water eluate, then eluted with 3 times the column volume of 30% ethanol, collected The eluate was concentrated to dryness under reduced pressure to obtain 3.8 g of concentrate. Mix the sample with 3 g of normal-phase column chromatography silica gel, evaporate the solvent, and take another 120 g of normal-phase column chromatography silica gel, and use the chloroform-methanol wet method with a volume ratio of 15:1 to install on an ordinary glass chromatography column, add the sample, First use chl...

Embodiment 2

[0025] Take the traditional Chinese medicine Cornus officinalis, crush it, pass through a 40-mesh sieve, accurately weigh 200 g, and heat and reflux with 1800 mL of 65% ethanol to extract twice, 40 minutes each time. The combined extracts were filtered, and the filtrate was concentrated under reduced pressure to obtain 102.7 g of the total extract. The total extract was dissolved in 100 mL of pure water, filtered, and the filtrate was placed on a macroporous adsorption resin column. First eluted with 1 column volume of water, discarded the water eluent, then eluted with 3 column volumes of 30% ethanol, collected the eluate, concentrated to dryness under reduced pressure, and obtained 14.3 g of a concentrate. Mix the sample with 14 g of normal-phase column chromatography silica gel, evaporate the solvent, and take another 450 g of normal-phase column chromatography silica gel, wet-pack the column with chloroform-methanol with a volume ratio of 15:1 on an ordinary glass chromato...

Embodiment 3

[0027] Take the traditional Chinese medicine Cornus officinalis, crush it, pass through a 40-mesh sieve, accurately weigh 5.0 kg, and extract twice with 40 L of 65% ethanol under reflux, 40 minutes each time. The combined extracts were filtered, and the filtrate was concentrated under reduced pressure to obtain a total extract of 2.4 kg. The total extract was dissolved in 2 L of pure water, filtered, and the filtrate was applied to a macroporous adsorption resin column. First elute with 1 column volume of water, discard the water eluent, then elute with 3 column volumes of 30% ethanol, collect the eluate, and concentrate to dryness under reduced pressure to obtain a concentrate of 0.36 kg. Mix the sample with 300 g of normal-phase column chromatography silica gel, evaporate the solvent, and take another 10 kg of normal-phase column chromatography silica gel, wet-pack the column with chloroform-methanol with a volume ratio of 15:1 on an ordinary glass chromatography column, add...

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Abstract

The invention discloses a method for preparation of loganin from Cornus officinalis. The method uses traditional Chinese medicine Cornus officinalis as a raw material, and comprises the steps of ethanol heating extraction, macroporous adsorption resin purification, silica gel column chromatography separation, and recrystallization, so as to obtain loganin with purity greater than 95% and extraction of 70.5-75.2%.

Description

technical field [0001] The invention relates to the technical field of traditional Chinese medicines, in particular to a method for preparing iridoid glycoside active substances from the traditional Chinese medicine Cornus officinalis. Background technique [0002] Dogwood ( Cornus officinalis Sieb. & Zucc.) is a deciduous tree or shrub of the genus Cornus in the family Cornaceae, widely distributed in Shanxi, Shaanxi, Gansu, Shandong, Jiangsu, Zhejiang, Anhui, Jiangxi, Henan, Hunan and other places, and also distributed in Korea and Japan. Its dry and mature pulp is the traditional Chinese medicine Cornus officinalis, also known as cornus, cornus, etc., which is recorded in the 2010 edition of "Chinese Pharmacopoeia", and is used to treat dizziness, tinnitus, waist and knee pain, impotence, nocturnal emission, enuresis, frequent urination, metrorrhagia, Profuse sweating, profuse thirst, internal heat, etc. It is widely used clinically, and is a variety of compound or pat...

Claims

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Application Information

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IPC IPC(8): C07H17/04C07H1/08
CPCC07H17/04C07H1/08
Inventor 师彦平解笑瑜陈娟
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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