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Method for simultaneously preparing high-purity morroniside and loganin from cornus officinalis extract

A technology of loganin and loganin, which is applied in the field of the simultaneous preparation of high-purity morroniside and loganin from logiflora extract, and achieves the effects of rapid separation and recovery, simple and easy operation, and high efficiency.

Active Publication Date: 2021-01-22
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 overcome the shortcomings of the simultaneous preparation of purified morroniside and loganin in the existing preparation methods and technologies, and propose a preparation method that is simple, easy to operate, high in yield and suitable for large-scale production and simultaneous preparation Method for high purity morroniside and loganin

Method used

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  • Method for simultaneously preparing high-purity morroniside and loganin from cornus officinalis extract
  • Method for simultaneously preparing high-purity morroniside and loganin from cornus officinalis extract

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The extraction of the fruit of cornus officinalis of embodiment 1

[0033] 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 for ultrasonic extraction. The power of the ultrasonic wave was 300W, and the extraction time was 60min. Continuously extracted three times, combined the extracts, and decompressed Concentrate and dry to get the extract of Cornus officinalis.

Embodiment 2

[0034] Embodiment 2 Preparation of high-purity morroniside and loganin

[0035] 1) Macroporous adsorption resin enrichment

[0036] The cornus officinalis extract was dissolved in water and filtered to obtain the filtrate. The filtrate was loaded onto HP-20 macroporous adsorption resin column by wet method, and after the sample was completely absorbed, it was sequentially eluted with pure water, 10%, 40%, 70%, and 95% ethanol, and the eluate was collected. 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.

[0037] 2) Normal phase silica gel column separation

[0038] Take 500g of the above-mentioned dry matter, dissolve it with 5000ml of methanol, mix the sample with normal phase silica gel (160-200 mesh); use normal ...

Embodiment 3

[0043] Embodiment 3 HPLC detection method

[0044] Liquid chromatograph: Waters2545 type 2998 ultraviolet detector

[0045] Chromatographic column: Waters sunfire C18Column (4.6×250mm, 5μm)

[0046] Mobile phase: methanol: water = 30:70

[0047] Flow rate: 1mL / min

[0048] Detection wavelength: 240nm

[0049] Injection volume: 10μl

[0050] Peaking time: 9.22min for morroniside and 20.92min for loganin

[0051] Preparation solution of the test sample and reference substance: dissolved in chromatographic grade methanol.

[0052] Using the above-mentioned instruments and methods, the morroniside and loganin obtained in Example 2 are detected, and the HPLC chromatograms for the purity inspection of morroniside and loganin are as follows: figure 1 and figure 2 As shown, compared with the spectrum of the reference substance, it was determined to be morroniside and loganin monomers, and the purity was ≧98%.

[0053] In the present invention, the extract of Cornus officinali...

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Abstract

The invention relates to a method for simultaneously preparing high-purity morroniside and high-purity loganin from dogwood extract. The method comprises the following steps: performing macroporous adsorption resin enrichment and normal phase silica gel preliminary separation on the dogwood extract, then performing treatment by a medium-pressure reverse phase silica gel chromatographic column, performing gradient elution by taking ethanol and water as a mobile phase, mixing the same components, and performing concentration under reduced pressure to respectively obtain a morroniside crude product of which the purity is greater than or equal to 90% and a loganin crude product of which the purity is greater than or equal to 90%; and respectively performing purification with a Sephadex LH-20 gel column, performing elution by adopting a chloroform and methanol mixed solvent, mixing the same components, and performing evaporation to dryness under reduced pressure to obtain the high-purity morroniside and the high-purity loganin. The method is simple and easy in operation and mild in conditions and is suitable for simultaneously preparing and producing morroniside of which the purity is greater than or equal to 98% and loganin of which the purity is greater than or equal to 98% in a large scale from the dogwood extract.

Description

technical field [0001] The invention relates to a method for simultaneously preparing high-purity morroniside and loganin from an extract of Cornus officinalis, in particular to a medium-pressure reversed-phase silica gel column chromatography combined with Sephadex, which has a significant separation effect on morroniside and loganin LH-20 (Hydroxypropyl Sephadex) Gel Column Chromatography for the separation of high-purity target compounds. Background technique [0002] Cornus officinalis is a plant of the genus Cornus officinalis Sieb.Et Zucc. in the family Cornaceae. Its medicinal parts are dried and mature pulp, which has the effect of nourishing the liver and kidney, and astringent and solidifying. Diabetes, etc., are widely used. There are a variety of chemical components in Cornus officinalis, and iridoid glycosides are the main active components, while morroniside and loganin are the two components with the largest content in the total iridoid glycosides, and they a...

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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