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Method for preparing loganin from cornus officinalis extract

A technology of strychnine and cornus, which is applied in the field of preparation of strychnine from the extract of cornus

Active Publication Date: 2021-02-26
BEIJING UNION UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to address the deficiencies in the preparation of purified loganin in the existing preparation methods and technologies, and propose a method for preparing high-purity loganin with a simple preparation method, easy operation, high yield and suitable for large-scale production

Method used

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  • Method for preparing loganin from cornus officinalis extract

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1 Extraction of the fruit of Cornus officinalis

[0031] Pulverize 10 kg of dried cornus fruit through a 20-mesh sieve, use 50% ethanol as a solvent, and perform ultrasonic extraction with a liquid-to-material ratio of 10:1. The power of the ultrasonic wave is 300 W, and the extraction time is 60 min. Continuous extraction is performed three times, the extracts are combined, and the pressure is reduced. Concentrated and dried to obtain Cornus officinalis extract.

Embodiment 2

[0032] The preparation of embodiment 2 high-purity loganin

[0033] 1) Macroporous adsorption resin enrichment

[0034] The dogwood extract was dissolved in water and filtered to obtain a filtrate. The filtrate was wet-loaded onto HP-20 macroporous adsorption resin column, and after the sample was completely adsorbed, it was sequentially eluted with pure water, 10%, 40%, 70%, and 95% ethanol gradient to collect the eluate. The flow rate was 40 ml / min with 3 column volumes per gradient. According to the detection of thin layer and high performance liquid chromatography, the target substances are all enriched in the eluted part of 40% ethanol, and the eluted part of 40% ethanol is concentrated and dried under reduced pressure.

[0035] 2) Normal phase silica gel column separation

[0036]Take 500 g of the above dried product, dissolve it in 5000 ml of methanol, and mix the sample with normal phase silica gel (160-200 mesh); use atmospheric pressure silica gel column chromatog...

Embodiment 3

[0041] Example 3 HPLC detection method

[0042] Liquid Chromatograph: Waters 2545 Model 2998 UV Detector

[0043] Chromatographic column: Waters sunfire C18Column (4.6×250mm, 5μm)

[0044] Mobile phase: methanol: water = 30:70

[0045] Flow rate: 1mL / min

[0046] Detection wavelength: 240nm

[0047] Injection volume: 10μl

[0048] Peak time: 20.92min

[0049] Preparation solution for the test product and reference substance: dissolve in chromatographic grade methanol.

[0050] Adopt above-mentioned instrument and method, the logariside that embodiment 2 obtains is detected, logariside purity checks HPLC chromatogram such as figure 1 As shown, it was determined to be loganin monomer by comparison with the reference substance, and the purity was ≧98%.

[0051] In the present invention, the Cornus officinalis extract is preliminarily separated by macroporous adsorption resin and normal-phase silica gel, and then separated by medium-pressure reversed-phase silica gel. Conc...

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Abstract

The invention relates to a method for preparing high-purity loganin from cornus officinalis extract. After the extract of Cornus officinalis was enriched by macroporous adsorption resin and preliminarily separated by normal phase silica gel, the sample containing loganin was passed through a medium-pressure reversed-phase silica gel chromatography column, and the mobile phase was ethanol and water for gradient elution, and the samples rich in loganin The eluent of glycoside was concentrated under reduced pressure to obtain crude loganin with a purity of ≥ 90%; finally, it was purified by Sephadex LH‑20 gel column chromatography, eluted with a mixed solvent of chloroform and methanol, and the eluent was evaporated under reduced pressure. Dry to obtain loganin with a purity of ≧98%. The method has remarkable separation effect, high speed and high efficiency, simple operation and mild conditions.

Description

technical field [0001] The present invention relates to a method for preparing high-purity loganin from cornus officinalis extract, in particular to a medium-pressure reversed-phase silica gel column chromatography with significant separation and purification effect on loganin, combined with Sephadex LH-20 (hydroxypropyl glucoside) Separation method for preparing high-purity target compounds by Sephadex) gel column chromatography. Background technique [0002] Dogwood is the dried and mature pulp of the genus Cornus in the family Cornelaceae, and is a Chinese medicinal material that can be used both medicinally and edible. Modern pharmacological studies have shown that it has pharmacological effects such as anti-senile dementia, anti-tumor, cardiovascular protection, and immune regulation. Loganin is a component with a relatively high content in total iridoid glycosides of Cornus officinalis. It has good activities in cardiovascular protection and immune regulation, and is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/04C07H1/08
CPCC07H1/08C07H17/04
Inventor 王欣尚小雅李金杰栾娜戴雪伶
Owner BEIJING UNION UNIVERSITY
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