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Preparation and application of active ingredients of Ligustrum lucidum

A signal suppression and glutamic acid technology, applied in the field of medicine, can solve problems such as unfavorable environmental protection, water pollution, complicated operation, etc., and achieve the effects of less environmental pollution, improved yield and purity, and simple operation.

Inactive Publication Date: 2017-05-10
朱海生 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is also the problem of complicated operation and low yield
And petroleum ether, CHCl 3 , EtOAc are toxic solvents, easy to cause water pollution, not conducive to environmental protection

Method used

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  • Preparation and application of active ingredients of Ligustrum lucidum
  • Preparation and application of active ingredients of Ligustrum lucidum
  • Preparation and application of active ingredients of Ligustrum lucidum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Example 1: Preparation of cosmoside and privet acid

[0056] 5kg of Ligustrum lucidum collected in November, dried in the sun, crushed to about 10 meshes, extracted twice with 50kg of 80% (v / v) ethanol under reflux, each time for 3 hours, combined extracts, concentrated under reduced pressure until alcohol-free After standing overnight, it was applied to DIAION HP20 macroporous adsorption resin, and then eluted with 3 times the volume of water, 3 times the volume of 15% ethanol, and 5 times the volume of 75% ethanol. Among them, the 75% ethanol eluted part was concentrated under reduced pressure, and the solvent was recovered to obtain a suspension. The obtained suspension was dissolved by adding 1 / 4 volume of 95% ethanol, the solution was preliminarily separated by polyamide column, ethanol gradient elution, TLC detection, according to cosmoside standard and privet acid standard, the eluate was collected, respectively An eluate containing cosmoside and an eluate conta...

Embodiment 2

[0061] Example 2: Preparation of cosmoside and privet acid

[0062] 4kg of Ligustrum lucidum collected in December, dried in the sun, crushed to about 10 mesh, soaked and extracted with 40kg of 75% (v / v) ethanol for 3 times, each time for 12h, combined extracts, concentrated under reduced pressure until no alcohol smell After standing overnight, apply AMBERLITE XAD16N macroporous adsorption resin, and then use 3 times the volume of water, 3 times the volume of 15% ethanol, and 5 times the volume of 75% ethanol to elute. The 75% ethanol eluate was concentrated under reduced pressure to obtain a suspension. The resulting suspension was dissolved by adding 1 / 4 volume of 95% ethanol, separated by Sephadex LH20 column chromatography, eluted with 80% methanol, and detected by TLC. The eluate containing cosmoside and the eluate containing privet acid were respectively obtained.

[0063] The eluate containing cosmoside was concentrated to a small amount of liquid, left to stand over...

Embodiment 3

[0065] Example 3: Preparation of cosmoside and privet acid

[0066] 3kg of Ligustrum lucidum collected in December, dried in the sun, crushed to about 10 meshes, soaked and extracted with 30kg of 75% (v / v) ethanol twice, each time for 48h, combined extracts, concentrated under reduced pressure until no alcohol smell After standing overnight, apply D101 macroporous adsorption resin, and then use 3 times the volume of water, 3 times the volume of 15% ethanol, and 5 times the volume of 75% ethanol to elute. The 75% ethanol eluate was concentrated under reduced pressure, and the solvent was recovered to obtain a suspension. After ODS column chromatography, 30-90% methanol gradient elution, according to the peak time of the standard cosmoside and privet acid standard, collect the eluate, and obtain the eluate containing cosmoside and the eluate respectively. Eluent containing privet acid.

[0067] The eluate containing cosmoside was purified by a medium-pressure preparative colum...

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Abstract

The invention belongs to the technical field of medicine and discloses preparation of cosmosiin and nuezhenidic acid in glossy privet fruit and application of two active ingredients. A method for preparing cosmosiin and nuezhenidic acid comprises the following steps: after drying and grinding glossy privet fruit, carrying out refluxing extraction or quenching extraction by hydrous ethanol; carrying out adsorption on extracting solution by macroporous adsorption resin and carrying out elution on the extracting solution by hydrous ethanol; after steaming eluent to remove a solvent, purifying the eluent by a chromatographic column, and according to cosmosiin standards and nuezhenidic acid standards, collecting eluent to respectively obtain eluent comprising cosmosiin and eluent comprising nuezhenidic acid; then respectively purifying to prepare the cosmosiin and the nuezhenidic acid. Compared with the prior art, the preparation method disclosed by the invention is simple and rapid to operate and also can be used for carrying out mass production; compared with those in a conventional method, both yield and purity of the prepared cosmosiin and nuezhenidic acid are obviously improved; the prepared cosmosiin and nuezhenidic acid are suitable for industrial production; moreover, a toxic organic solvent is avoided being used, and the preparation method is safe and environmental-friendly.

Description

technical field [0001] The invention belongs to the technical field of medicine, and specifically relates to the preparation and application of active components of Ligustrum lucidum, especially the preparation of cosmoside and privet acid in Ligustrum lucidum and the application of the two active components. Background technique [0002] Ligustrum lucidum is the dry mature fruit of Ligustrum lucidum Ait (Oleaeeae) plant, listed as top grade in "Shen Nong's Materia Medica", and is a traditional Chinese medicine for strengthening the body and strengthening the roots. Ligustrum lucidum tastes sweet, bitter, cool in nature, has the effect of nourishing the liver and kidney, improving eyesight and black hair. Clinically, it is mainly used to treat dizziness and tinnitus, soreness of waist and knees, dark eyes, premature graying of beard and hair, etc. [0003] For a long time, the fat-soluble triterpene acids represented by oleanolic acid in Ligustrum lucidum have been deeply a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/07C07H17/04C07H1/08A61K31/7048A61P25/00A61P39/06A61P43/00
Inventor 朱海生王文
Owner 朱海生