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Preparative chromatographic separation of compounds in Oxytropis based on parallel separation mode

A separation mode and technology for separating Oxytropis, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve the problem of lack of systematic and in-depth research on the mechanism of action of active substances in Oxytropis and the inability to meet the needs of new drug creation in Oxytropis Quality control requirements, restrictions on the development and research of Oxytropis medicinal materials, etc., to achieve the effects of rapid separation and preparation, increased chemical production, and easy promotion

Active Publication Date: 2018-04-06
CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, scholars from various countries have isolated more than 140 compounds from more than 20 medicinal plants of the genus Oxytropis, most of which are flavonoids, triterpenoids and alkaloids, and there is no systematic and in-depth study of the active substances in Oxytropis. mechanism of action, only preliminary pharmacological activity studies have been conducted
At the same time, it is also impossible to stably obtain chemical reference substances with a purity of more than 98%, which cannot meet the quality control requirements for the creation of new drugs and related preparations of Oxytropis chinensis, thus restricting the medicinal development and research of Oxytropis chinensis medicinal materials

Method used

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  • Preparative chromatographic separation of compounds in Oxytropis based on parallel separation mode
  • Preparative chromatographic separation of compounds in Oxytropis based on parallel separation mode
  • Preparative chromatographic separation of compounds in Oxytropis based on parallel separation mode

Examples

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Effect test

Embodiment 1

[0053] Example 1 Preparation of a method for chromatographically separating compounds in Oxytropis chinensis based on parallel separation mode, comprising the following steps:

[0054] ⑴ Preparation of Oxytropis extractum:

[0055] The Oxytropis falciparum was subjected to microwave extraction with 5% ethanol to obtain the extract; the extract was concentrated under reduced pressure at a pressure of 0.02 MPa to obtain the Oxytropis extract extract.

[0056] Among them: the conditions of microwave extraction refer to the ratio of solid to liquid: 1 g: 5 mL, the extraction temperature is 60 °C, the number of extractions is 1 time, each time 1 h, and the microwave power is 1 KW.

[0057] ⑵Extraction:

[0058] After dissolving the Oxytropis extract extract in deionized water with 1 times its mass, it was extracted with petroleum ether and ethyl acetate in sequence to obtain petroleum ether fraction, ethyl acetate fraction and water fraction respectively.

[0059] (3) The water par...

Embodiment 2

[0069] Example 2 Preparation of a method for chromatographic separation of compounds in Oxytropis chinensis based on parallel separation mode, comprising the following steps:

[0070] ⑴ Preparation of Oxytropis extractum:

[0071] The Oxytropis gansuensis was subjected to microwave extraction with ethanol with a volume concentration of 95% to obtain an extract; the extract was concentrated under reduced pressure at a pressure of 0.07MPa to obtain the Oxytropis extract extract.

[0072] Among them: the conditions of microwave extraction refer to the ratio of solid to liquid: 1 g: 30 mL, the extraction temperature is 95 °C, the extraction times are 4 times, 4 h each time, and the microwave power is 100KW.

[0073] ⑵Extraction:

[0074] The Oxytropis extract extract was dissolved in deionized water 10 times its mass, and then extracted with petroleum ether and ethyl acetate in sequence to obtain petroleum ether fractions, ethyl acetate fractions and water fractions, respectively...

Embodiment 3

[0084] Example 3 Preparation of a method for chromatographic separation of compounds in Oxytropis chinensis based on parallel separation mode, comprising the following steps:

[0085] ⑴ Preparation of Oxytropis extractum:

[0086] The Oxytropis multi-leaf was extracted by microwave with 5% methanol to obtain the extract; the extract was concentrated under reduced pressure at a pressure of 0.06MPa to obtain the Oxytropis extract extract.

[0087] Among them: the conditions of microwave extraction refer to the solid-liquid ratio of 1 g: 15 mL, the extraction temperature of 75 °C, the extraction times of 3 times, each time of 3 h, and the microwave power of 60KW.

[0088] ⑵Extraction:

[0089] The Oxytropis extract extract was dissolved in deionized water six times its mass, and then extracted with petroleum ether and ethyl acetate in sequence to obtain the petroleum ether fraction, ethyl acetate fraction and water fraction, respectively.

[0090] (3) The water part is injected...

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Abstract

The invention relates to a method for separating a new compound from whin based on parallel separation type preparative chromatography. The method comprises the following steps of: (1) preparing whin extractum: carrying out alcohol extraction and reduced-pressure concentration on whin to obtain the whin extractum; (2) extracting: dissolving the whin extractum and extracting to obtain a petroleum ether part, an ethyl acetate part and a water part; (3) injecting the water part to a macroporous resin column and eluting to obtain 20%, 40%, 60% and 80% elution parts; (4) drying 40% ethanol part to constant weight to obtain 40% ethanol part dry powder; and (5) dissolving the 40% ethanol part dry powder, injecting to a preparative chromatographic device with a parallel separation mode, and carrying out primary and secondary separation, elution and online ultraviolet detection to obtain the new compound kaempferol 3-O-a-L-rhamnopyranosyl-(1 to 2)-[6-O-(3-hydroxy-3-methylglutaryl)-b-D-glucopyranoside] which meets the chemical control requirement and has purity more than 98%. The method has simple process, high repeatability and high recovery.

Description

technical field [0001] The invention relates to a preparation method of a compound, in particular to a method for preparing a chromatographically separated compound in Oxytropis chinensis based on a parallel separation mode. Background technique [0002] Oxytropis ( Oxytropis D.C.) The plant belongs to the subfamily Fabaceae Papilionaceae. This genus is a perennial herb, semi-shrub or shrub, and there are more than 300 species in the world. In my country, there are 131 species of Oxytropis (more than 20 species of medicinal plants), which are distributed in Gansu, Qinghai, Inner Mongolia, Sichuan, Tibet and other places. The medicinal plants of the genus Oxytropis were recorded in the 1977 edition of the Chinese Pharmacopoeia. It is widely distributed in my country and is often used in compound prescriptions of Tibetan and Mongolian medicines. [0003] Tibetan medicine Oxytropis ( Oxytropis falcate Bunge) (Tibetan medicine named Er Daxia) is a legume ( Leguminosae ) O...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/07C07H1/08
CPCC07H1/08C07H17/07
Inventor 陈晨李玉林刘凤芹
Owner CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST