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Compounds A and B extracted from Common Macrocarpium Fruit as well as preparation method and application of same

A technology for compounds and compounds, applied in the field of medicine, can solve problems such as no public reports

Pending Publication Date: 2021-05-18
HENAN UNIV OF CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Following the ancient medicine habits, combined with the previous research on Cornus officinalis, it is hoped to obtain new compounds with novel structure and strong anti-inflammatory activity from Cornus officinalis, which can be effectively used in the treatment of rheumatoid arthritis, but there has been no public report so far

Method used

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  • Compounds A and B extracted from Common Macrocarpium Fruit as well as preparation method and application of same
  • Compounds A and B extracted from Common Macrocarpium Fruit as well as preparation method and application of same
  • Compounds A and B extracted from Common Macrocarpium Fruit as well as preparation method and application of same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A pair of compound A and compound B extracted from Fructus officinalis of the present invention, its structural formula is respectively:

[0031]

[0032] Its preparation method comprises the following steps:

[0033] (1) Take 5kg of dried Cornus officinalis, add 40L of water each time, boil and extract at 100°C for 3 times, extract for 2.h each time, combine the extracts, and concentrate under reduced pressure to a concentrated solution equivalent to 1.1g / mL of crude drug;

[0034] (2) Load the concentrated solution on a D101 macroporous adsorption resin column with a diameter-to-height ratio of 1:10, and carry out gradient elution with 36 L of water and 36 L of ethanol (30% EtOH) with a volume concentration of 30% in sequence, at a flow rate of 4 mL / min. The eluate from 30% ethanol was concentrated under reduced pressure to obtain the extract Fr. with a relative density of 1.3 at 50°C. 30％EtOH (the first extract, 230g);

[0035] (3) Extract Fr. 30％EtOH Separatio...

Embodiment 2

[0039] A pair of preparation methods of Compound A and Compound B extracted from Cornus officinalis of the present invention comprise the following steps:

[0040] (1) Take 5kg of dried Cornus officinalis, add 50L of water each time, boil and extract at 100°C for 3 times, extract for 3 hours each time, combine the extracts, and concentrate under reduced pressure to a concentrated solution equivalent to 1.2g / mL of crude drug;

[0041] (2) Load the concentrated solution on a D101 macroporous adsorption resin column with a diameter-to-height ratio of 1:6, and perform gradient elution with 18 L of water and 48 L of ethanol with a volume concentration of 30% in sequence at a flow rate of 4 mL / min. Deliquified, concentrated under reduced pressure to obtain the extract Fr. 30％EtOH (the first extract 250g);

[0042] (3) Extract Fr. 30％EtOH Separation by 300-mesh silica gel column chromatography, r=4cm, H=12cm, gradient elution (natural flow rate) with volume ratios of 100:0, 100:2, ...

Embodiment 3

[0046] A pair of preparation methods of Compound A and Compound B extracted from Cornus officinalis of the present invention comprise the following steps:

[0047] (1) Take 5kg of dried Cornus officinalis, add 80L of water each time, boil and extract 5 times at 100°C for 2.5 hours each time, combine the extracts, and concentrate under reduced pressure to a concentrated solution equivalent to 1.2g / mL of crude drug;

[0048] (2) Load the concentrated solution on a D101 macroporous adsorption resin column with a diameter-to-height ratio of 1:4, and perform gradient elution with 12 L of water and 33 L of ethanol with a volume concentration of 30% in sequence at a flow rate of 3 mL / min. Deliquified, concentrated under reduced pressure to obtain the extract Fr. with relative density 1.35 at 50°C 30％EtOH (the first extract 280g);

[0049] (3) Extract Fr. 30％EtOH Separation by 300 mesh silica gel column chromatography, r=5cm, H=18cm, gradient elution (natural flow rate) with volume ...

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Abstract

The invention relates to compounds A and B extracted from Common Macrocarpium Fruit as well as a preparation method and application thereof, which can effectively solve the problems of preparation of new compounds A and B from Common Macrocarpium Fruit and application in preparation of anti-inflammatory drugs. The method includes steps that water is added into Common Macrocarpium Fruit for boiling extraction, wherein the extract is concentrated under reduced pressure, the concentrated extract is loaded on a D101 macroporous adsorption resin column, elution is carried out with water and 30% ethanol in sequence, and the 30% ethanol part eluent is collected; then vacuum concentration is carried out to obtain an extract Fr.30% EtOH, and silica gel column chromatography separation and dichloromethane-methanol gradient elution are performed to collect a 100:5 eluent; vacuum concentration is carried out toobtain an extract Fr.30% EtOH-4; ODS column chromatography separation and then vacuum gradient elution with methanol-water are carried out to collect a 30: 70 eluent, and then vacuum concentration is carried out to obtain an extract Fr.30% EtOH-4-3; and Sephadex LH-20 column chromatography separation is conducted, methanol elution is carried out, the solvent is recovered under reduced pressure, and recrystallization is performed to obtain the compounds A and B. The method is easy to operate, high in guidance quality and high in product purity, the compound can be effectively used for preparing the anti-inflammatory medicine, and the new application and the medicinal value of the Common Macrocarpium Fruit are developed.

Description

technical field [0001] The invention relates to medicine, in particular to a pair of compounds A and B extracted from Cornus officinalis and its preparation method and application. Background technique [0002] Cornus officinalis is the dried and mature pulp of Cornus officinalis Sieb. et Zucc., a plant of the family Cornaceae. It has been used in medicine for more than two thousand years in our country, and it was first recorded in "Shen Nong's Materia Medica". "It has the effects of nourishing the liver and kidney, astringent essence and detoxification, etc., and was listed as a traditional Chinese medicine with the same origin of medicine and food in my country in 2018. Henan, Shaanxi and Zhejiang are the three main producing areas of dogwood, among which the cornus produced in Henan accounts for more than 60% of the total output, with an annual output of more than 4,000 tons and an annual demand of more than 5,000-6,000 tons. In clinical treatment and classic prescripti...

Claims

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Application Information

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IPC IPC(8): C07D307/88A61K31/365A61P19/02A61P29/00
CPCC07D307/88A61P19/02A61P29/00C07B2200/07Y02A50/30
Inventor 代丽萍李红彬冯庆梅许二平王智民张玲霞张丽萍
Owner HENAN UNIV OF CHINESE MEDICINE
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