Preparation method of cornuside bulk drug

A technology of new glycosides and raw materials of Cornus officinalis, which is applied in the field of biomedicine, can solve the problems of high equipment requirements, high cost, and large equipment investment, and achieve high purity, high yield, and simple and practical process

Pending Publication Date: 2021-10-08
BEIJING UNIV OF CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The defect of this method is that: 1) the new glycosides of Cornus officinalis are not separated, and the crude extract of the cyclene glycosides of Cornus officinalis is obtained, which also includes some large amounts of cyclic glycosides such as morroniside, loganin, swertigin, etc. 2) The preparation process requires high equipment, large equipment investment and high cost; 3) There is no industrial-grade equipment for ultrasonic extraction, which cannot be produced on a large scale and industrially

Method used

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  • Preparation method of cornuside bulk drug
  • Preparation method of cornuside bulk drug
  • Preparation method of cornuside bulk drug

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Crushing the causing fruit into powder, add concentration of 50% ethanol to extract several times (for example, 2-4 times, 2-4h each time), combined extract, filtrate, concentrate to nano, concentrate liquid;

[0037] (2) After adding the above concentrated liquid, then extracts several times (e.g., 2-4 times) with ethyl acetate, combined with aqueous phase, concentrated under reduced pressure, and the water concentrate after extracting;

[0038] (3) The water concentrate after extraction is slowly absorbed in the D101 macroporous adsorption resin column, the wet mounting column (the amount ratio of the sample and the column resin is 1: 5), first elution of 6bV with 35% ethanol, discard After 55% ethanol eluting with 5BV, the eluate is collected into one-third or quarter of one-quarter, and the eluent containing halophysin is collected by thin layer chromatography or HPLC. The concentrate is concentrated under reduced pressure (the relative density is 1.15); in the conc...

Embodiment 2

[0043] (1) Crushing the causing fruit into powder, add concentration of 40% ethanol to reflux (for example, 2-4 times, 2-4h each time), combined extract, filtrate, concentrate concentration to nano, concentrate liquid;

[0044] (2) After adding the above concentrated liquid, then extracts several times (e.g., 2-4 times) with ethyl acetate, combined with aqueous phase, concentrated under reduced pressure, and the water concentrate after extracting;

[0045] (3) The water concentrate after extraction is slowly sampled in the AB-8 macroporous adsorption resin column, the wet mounting column (the amount of the sample and the amount of the column resin is 1: 5), first elution of 6bV with 35% ethanol, Abandon; eluate 55% ethanol, eluent is collected in one-third or quarter of one-quarter, with silica gel layer chromatography or HPLC, collect the elution of hawthorn Liquid, concentrate concentrate (1.10) under reduced pressure (density is 1.10); in the concentrate in 60-100 alcohol-solub...

Embodiment 3

[0048] (1) Crushing the fruits of the hawthorn into coarse powder, add 60% ethanol to extract several times (for example, 2-4 times, 3 hours each time), combined with extract, filtrate, concentrate to nano, concentrate;

[0049] (2) After adding the above concentrated liquid, then extracts several times (e.g., 2-4 times) with ethyl acetate, combined with aqueous phase, concentrated under reduced pressure, and the water concentrate after extracting;

[0050] (3) The water concentrate after extraction is slowly sampled in the HP-20 macroporous adsorption resin column, the wet mounting column (the amount ratio of the sample and the column resin is 1: 5), first elution of 6bV with 35% ethanol, Abandon; eluate 55% ethanol, eluent is collected in one-third or quarter of one-quarter, with silica gel layer chromatography or HPLC, collect the elution of hawthorn Liquid, concentrated concentrate (relative density of 1.13); in the concentrate in 60-100 alcohol-soluble polyamide resin columns...

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Abstract

The invention provides a preparation method of a cornuside bulk drug. The preparation method comprises the following steps: crushing dogwood fruits to obtain dogwood fruit powder, adding an extraction solvent into the dogwood fruit powder for reflux extraction to obtain an extracting solution, performing filtering, and performing vacuum concentration to obtain a concentrated solution; extracting the concentrated solution by using an organic solvent, and performing vacuum concentration to obtain an extracted water concentrated solution; sequentially carrying out macroporous adsorption resin column chromatography and polyamide resin column chromatography on the extracted water concentrated solution, then carrying out gradient elution by utilizing an elution solvent, carrying out silica gel thin-layer chromatography or high performance liquid chromatography(HPLC) inspection, collecting and combining an eluent containing cornuside, and carrying out vacuum concentration to obtain a cornuside concentrated solution; and finally, carrying out recrystallization treatment on the cornuside concentrated solution, and then performing drying to obtain the cornuside. The preparation method has a simple and practical technological process and low toxicity and is environment-friendly, and specific technological conditions are adopted in all the steps, so that high-yield and high-purity cornuside is obtained.

Description

Technical field [0001] The present invention relates to the field of biomedical technology, and more particularly to the preparation method of hawthorn cryptoside. Background technique [0002] At present, the Cornuside is a cycloolefin-based compound contained in the dry mature fruit of Cornusofficinalissieb.et Zucc., The structural formula is as follows: [0003] [0004] [CAS] 131189-57-6 [0005] [Molecular Formula and Molecular Weight] C 24 Hide 30 O 14 ; 542.49 [0006] [Physical and Chemical Properties] White powders, soluble in methanol, ethanol, acetone, dimethyl sulfoxide, slightly soluble in diethyl ether, is hard to dissolve in ethyl acetate, insoluble in petroleum ether. Bugue: -91 (C = 1.0 methanol); melting point: 108-109 ° C. [0007] The hawthorn cryptoside is a cycloolefin-based compound, which is one of the main components of traditional Chinese medicine hawthorn, with hypoglycemic, antiarrhythmic, inhibiting cytotoxicity, and other pharmacological activity. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08
CPCC07H17/04C07H1/08
Inventor 续洁琨张维库赫军连雯雯彭中灿张佳王泽星潘雪格
Owner BEIJING UNIV OF CHINESE MEDICINE
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