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Separation and preparation method for four glycoside chemical reference substances in Tibetan capillary artemisia

A technology for storing Yinchen and reference substances, which is applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., to achieve the effects of good stability and repeatability, shortening separation time, and reducing consumption of organic solvents

Inactive Publication Date: 2013-11-27
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

However, there are patents for the preparation of gentiopicroside, mangiferin, swertiroside and isoorientin with a purity of more than 98% by using preparative liquid chromatography, high-speed countercurrent chromatography and gel chromatography to simultaneously separate and prepare the chemical reference substances of gentiopicroside, mangiferin, and isoorientin from the medicinal material of Yinchen. Literature has not yet been reported

Method used

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  • Separation and preparation method for four glycoside chemical reference substances in Tibetan capillary artemisia
  • Separation and preparation method for four glycoside chemical reference substances in Tibetan capillary artemisia
  • Separation and preparation method for four glycoside chemical reference substances in Tibetan capillary artemisia

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Example 1 A method for isolating and preparing four kinds of glycoside chemical reference substances from Capum chinensis, comprising the following steps:

[0042] ⑴Preparation of extract extract:

[0043] Will hide Yin Chen medicinal material - Sichuan Swertia ( Swertia mussotii ) at a ratio of 1 g: 5 mL with ethanol with a volume concentration of 5% at an extraction temperature of 60°C, extraction times of 2 times, and extraction times of 1 h each time for heating and reflux extraction, and the extracts were combined; the extracts were extracted at a pressure of Under the condition of 0.02MPa, the extract of Capillary cypress extract was obtained after concentrating under reduced pressure.

[0044] ⑵Extraction:

[0045] After dissolving the extract extract of Yinchen chanterelles with 1 times its mass in deionized water, it was extracted with chloroform and n-butanol in sequence to obtain the chloroform fraction, n-butanol fraction and water fraction respective...

Embodiment 2

[0056] Example 2 A method for isolating and preparing four kinds of glycoside chemical reference substances from Capum chinensis, comprising the following steps:

[0057] ⑴Preparation of extract extract:

[0058] The Tibetan capillary herb - Swertia clam ( Swertia franchetiana ) at a ratio of 1 g: 30 mL with ethanol with a volume concentration of 95% at an extraction temperature of 95°C, extraction times of 4 times, and each time of 4 h for heating and reflux extraction, and the extracts were combined; the extracts were extracted at a pressure of Under the condition of 0.07MPa, the extract of Capillary cypress extract was obtained after concentrating under reduced pressure.

[0059] ⑵Extraction:

[0060] After dissolving the extract of Capillary root extract with 10 times its mass in deionized water, it was extracted with chloroform and n-butanol in sequence to obtain the chloroform fraction, n-butanol fraction and water fraction respectively.

[0061] (3) The n-but...

Embodiment 3

[0072] Example 3 A method for isolating and preparing four kinds of glycoside chemical reference substances from Capum chinensis, comprising the following steps:

[0073] ⑴Preparation of extract extract:

[0074] The Tibetan capillary herb - Swertia clam ( Swertia franchetiana ) at a ratio of 1 g: 20 mL with methanol at a volume concentration of 5% at an extraction temperature of 75°C and extraction times of 3 times for 2 h each time for heating and reflux extraction, and the extracts were combined; the extracts were extracted at a pressure of Under the condition of 0.05MPa, the extract of Capillary cypress extract was obtained after concentrating under reduced pressure.

[0075] ⑵Extraction:

[0076] After dissolving the extract extract of Yinchen chanterelles with 5 times its mass in deionized water, it was extracted with chloroform and n-butanol in sequence to obtain the chloroform part, n-butanol part and water part respectively.

[0077] (3) The n-butanol fract...

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Abstract

The invention relates to a separation and preparation method for four glycoside chemical reference substances in Tibetan capillary artemisia. The method comprises steps of (1) subjecting a Tibetan capillary artemisia medicinal material to alcohol extraction and concentration to obtain a Tibetan capillary artemisia extract; (2) extracting with chloroform and n-butanol separately, after the Tibetan capillary artemisia extract is dissolved, to obtain a chloroform part, an n-butanol part and a water part; (3) drying the n-butanol part to obtain dry powder of the n-butanol part; (4) dissolving the dry powder of the n-butanol part and injecting into a preparative high-performance liquid chromatography, and obtaining a component group of the four compounds after elution, on-line ultraviolet detection and drying; (5) pumping the stationary phase and the mobile phase of a solvent system into a high-speed countercurrent chromatography, and separating the component group, after the high-speed countercurrent chromatography is balanced, to obtain a four-glycoside mixture with a purity larger than 90%; and (6) dissolving the mixture, adding into a gel separation column, eluting and drying to obtain the four glycoside chemical reference substances with purities larger than 98%. The method is short in separation time, low in organic solvent consumption, and good in stability and repeatability.

Description

technical field [0001] The invention relates to a preparation method of a chemical reference substance, in particular to a method for separating and preparing four kinds of glycoside chemical reference substances from Capum chinensis. Background technique [0002] Tibetan Yinchen is used in Tibetan medicine to treat various diseases of the liver and gallbladder such as hepatitis, cholecystitis and gallbladder and jaundice. At present, it is impossible to stably obtain a chemical reference substance with a purity of more than 98% from Capillaris, which cannot meet the quality control requirements for the creation of new drugs and related preparations, which restricts the medicinal development and research of capillary. [0003] Scholars at home and abroad have also separated and purified the chemical components of gentiopicroside, mangiferin, swertigin, and isoorientin. For example, the patent CN102503996A has separated and purified gentiopicroside from Cape chinensis, but no...

Claims

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Application Information

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IPC IPC(8): C07H1/08C07H17/04C07D407/04
Inventor 陈晨李玉林陈涛孙菁
Owner CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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