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Method for preparing morroniside from cornus officinalis extract

A technology of Cornus officinalis and extract, applied in the field of preparation of morroniside from Cornus officinalis extract

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

AI Technical Summary

Problems solved by technology

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

Method used

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  • Method for preparing morroniside from cornus officinalis extract

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1 Extraction of Cornus officinalis Fruit

[0031] 10 kg of dried Cornus officinalis fruit was crushed through a 20-mesh sieve, the solvent was 50% ethanol, and the liquid-to-solid ratio was 10:1 (ml / g) for ultrasonic extraction, the power of the ultrasonic wave was 300W, and the extraction time was 60min. Continuously extracted three times, combined The extract was concentrated and dried under reduced pressure to obtain the cornus officinalis extract.

Embodiment 2

[0032] Embodiment 2 Preparation of high-purity morroniside

[0033] 1) Macroporous adsorption resin enrichment

[0034]The cornus officinalis extract was dissolved in water and filtered to obtain the filtrate. Pass the filtrate through HP-20 type macroporous adsorption resin column to make the sample completely adsorbed, then use pure water, 10%, 40%, 70%, 95% ethanol gradient elution successively, and collect the eluate. The flow rate was 40ml / min, and each gradient was eluted with 3 column volumes. According to thin-layer and high-performance liquid chromatography detection, the target substance is all enriched in the 40% ethanol elution site, and the 40% ethanol elution site is concentrated and dried under reduced pressure.

[0035] 2) Normal phase silica gel column separation

[0036] Take 500g of the above-mentioned dry matter, dissolve it in 5000ml of methanol, mix the sample with normal phase silica gel (160-200 mesh); use normal pressure silica gel column chromatogr...

Embodiment 3

[0041] Embodiment 3 HPLC detection method

[0042] Liquid chromatograph: Waters2545 type 2998 ultraviolet detector

[0043] Chromatographic column: Waters sunfire C18 Column (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: 9.22min

[0049] Preparation solution of the test sample and reference substance: dissolved in chromatographic grade methanol.

[0050] Using the above-mentioned instruments and methods, the morroniside obtained in Example 2 is detected, and the morroniside purity check HPLC chromatogram is as follows: figure 1 As shown, compared with the spectrum of the reference substance, it was determined to be morroniside monomer, and the purity was ≥98%.

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

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Abstract

The invention relates to a method for preparing high-purity morroniside from cornus officinalis extract. Cornus officinalis extract was enriched by macroporous adsorption resin and preliminarily separated by normal-phase silica gel, then passed through medium-pressure reverse-phase silica gel chromatography column, and the mobile phase was ethanol and water for gradient elution, and the eluent rich in morroniside was reduced Concentrate under reduced pressure to obtain crude morroniside with a purity of ≥90%; finally purify by Sephadex LH‑20 gel column chromatography, elute with a mixed solvent of chloroform and methanol, and evaporate the eluent to dryness under reduced pressure to obtain morroniside with a purity of ≥98%. Noroside. The method has remarkable separation effect, high speed and high efficiency, simple operation and mild conditions.

Description

technical field [0001] The invention relates to a method for preparing high-purity morroniside from an extract of Corni officinalis, in particular to a medium-pressure reversed-phase silica gel column chromatography which has a significant separation and purification effect on morroniside combined with Sephadex LH-20 (hydroxypropylglucose Glycan gel) separation method for preparing high-purity target compound by gel column chromatography. Background technique [0002] Cornus officinalis is a widely used traditional Chinese medicine, which has pharmacological effects such as anti-senile dementia, anti-tumor, and cardiovascular protection. Morroniside is one of the main components. Pharmacological studies have shown that morroniside has anti-inflammatory, anti-oxidant, and neuroprotective effects. Studies in recent years have shown that morroniside has excellent development and application potential in anti-senile dementia activity. Finding a simple and feasible method for p...

Claims

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Application Information

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