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A method for extraction, purification and detection of astragaloside in Beiqi mushroom

A technology of astragaloside and Beiqi mushroom, which is applied in the field of extraction, purification and inspection of active substances in Beiqi mushroom, can solve the problems of complex elution and enrichment, large measurement error, cumbersome operation, etc., and improve extraction efficiency and accuracy High, easy-to-operate effect

Inactive Publication Date: 2020-09-25
LULIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The content determination and detection of astragaloside have tried to use high performance liquid phase ultraviolet detector to detect, but because astragaloside has only weak absorption in the ultraviolet region, the solvent noise has a great influence on the result, the sensitivity is low, and the measurement error is large
Soxhlet reflux extraction requires alkali washing and macroporous resin enrichment process, the elution and enrichment are complicated and difficult to operate
In addition, there are water leaching method, alkaline water extraction method, reflux method, CO 2 Supercritical fluid extraction and other methods, but these methods have the disadvantages of less separation and purification, low precision, and large errors, and cannot achieve high-precision mass production
[0007] In order to solve the problems of complex operations and unreliable results in the extraction of astragaloside from Beiqi mushroom and the extraction and purification of astragalosides Ⅰ, Ⅱ, Ⅲ and astragaloside IV, the present invention provides a method that is easy to operate, takes short test time and has high extraction efficiency. A method for the extraction, purification and detection of astragaloside from Astragaloside prepared from microgram-level separation and analysis to gram-level separation and preparation

Method used

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  • A method for extraction, purification and detection of astragaloside in Beiqi mushroom
  • A method for extraction, purification and detection of astragaloside in Beiqi mushroom
  • A method for extraction, purification and detection of astragaloside in Beiqi mushroom

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Embodiment 1

[0062] Step a, crude extraction of astragaloside:

[0063] Dry Beiqi mushrooms in the shade in a ventilated place until the material becomes brittle, dry them in a constant temperature box (40-50°C), crush them with a high-speed multifunctional grinder, pass through an 80-mesh sieve, store them in a glass container, and accurately weigh 10.0 g Add 250mL of 70% ethanol to a 500mL Erlenmeyer flask, vibrate and extract in an air bath constant temperature oscillator at 50°C for 24 hours, fully soak and dissolve to form a crude extract;

[0064] The ultrasonic microwave extractor extracts in three stages, each stage is 5 minutes, a total of 15 minutes, select the best microwave ultrasonic conditions according to Table 1, extract under the condition of constant ultrasonic, set the temperature at 45 ° C, 50 ° C, 55 ° C, and finally measure the ultrasonic The power is 800, 900, 1000W, the microwave power is 250, 300, 350W is the best, the ultrasonic frequency is 50KHz, the mode is 15:...

Embodiment 2

[0102] Step a, crude extraction of astragaloside:

[0103] Dry Beiqi mushrooms in the shade in a ventilated place until the material becomes brittle, dry them in a constant temperature box (40-50°C), crush them with a high-speed multifunctional grinder, pass through an 80-mesh sieve, store them in a glass container, and accurately weigh 10.0 g Add 250mL of 70% ethanol to a 500mL Erlenmeyer flask, vibrate and extract in an air bath constant temperature oscillator at 50°C for 24 hours, fully soak and dissolve to form a crude extract;

[0104] The ultrasonic microwave extractor extracts in three stages, each stage is 5 minutes, a total of 15 minutes, select the best microwave ultrasonic conditions according to Table 4, extract under constant ultrasonic conditions, set the temperature at 45°C, 50°C, and 55°C, and finally measure the ultrasonic The power is 800, 900, 1000W, the microwave power is 250, 300, 350W is the best, the ultrasonic frequency is 50KHz, the mode is 15:10, the ...

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Abstract

The invention discloses a method for extracting, purifying, and inspecting astragalus in Beiqi mushrooms, and relates to the field of extraction, purification, and inspection of active substances in the Beiqi mushrooms. The method comprises the following steps of: taking 70% of ethanol as an extracting agent, and carrying out auxiliary treatment through a microwave ultrasonic auxiliary extractor to obtain an astragalus crude extracting solution; taking a mixed solution of chloroform, methanol, ethyl acetate, and water as a developing solvent, and separating and purifying astragaloside, astragalus saponin I, II, and III through thin-layer chromatography; using chromatography methanol and ultrapure water as a mobile phase, and accurately determining sample molecular mass information (a mass-to-charge ratio of molecular ions or fragment ions) with a high resolution mass spectrometer; detecting a functional group of the sample by infrared, and analyzing the molecular structure of the sample; and determining a rotation degree, a specific rotation degree, and a melting point of the sample. According to the method for extracting, purifying, and inspecting astragalus in Beiqi mushroom, microgram amount of separation analysis to gram amount of separation preparation can be achieved by using TLC-MS-IR series technology to detect astragalus in the Beiqi mushrooms; and the method is simpleto operate, short in time and high in efficiency.

Description

technical field [0001] The invention relates to the field of extraction, purification and inspection of active substances in Beiqi mushroom, in particular to a method for extracting, purifying and inspecting astragaloside in Beiqi mushroom. Background technique [0002] Beiqi mushroom, Pleurotus pleurotus under the Basidiomycota Agaricaceae, is a new type of Pleurotus pleurotus cultivated for many years by using Zhengbeiqi, a variety of Chinese herbal medicines and by-products of agricultural crops as culture materials, and adopting scientific formula and special technology. A new type of edible fungus developed in the selenium-rich area of ​​Hunyuan, Shanxi. According to the bioaccumulation effect, Beiqi mushroom contains the pharmacological components of Hunyuan Astragalus, which can enrich astragaloside to a certain extent during the growth and development process. Beiqi mushroom contains a variety of essential amino acids, polysaccharide proteins, antibiotics, taurine, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/90G01N30/94G01N30/95G01N30/06
CPCG01N30/06G01N30/90G01N30/94G01N30/95G01N2030/062
Inventor 杨卫民秦永其杜京旗张利军赵青红
Owner LULIANG UNIV
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