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Method for separating mannitol, adenosine and ergosterol in sample to be detected and application

A technology for ergosterol and mannitol, applied in the field of analysis and detection, can solve the problems of sample loss, long analysis time, time-consuming and labor-intensive, etc., and achieve the effects of improving grinding efficiency and improving dispersion uniformity.

Active Publication Date: 2020-09-01
DONGGUAN HEC CORDYCEPS R&D CO LTD +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the shortcomings of the existing technology of simultaneous determination of mannitol, adenosine and ergosterol in edible fungi, the defects of extraction and analysis time are long, and the existing technology of simultaneously separating and preparing ergosterol and adenosine from a medicinal material is time-consuming and laborious , loss of samples, the present invention establishes a method for synchronous preparation and rapid quantitative detection of mannitol, adenosine and ergosterol in edible fungi

Method used

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  • Method for separating mannitol, adenosine and ergosterol in sample to be detected and application
  • Method for separating mannitol, adenosine and ergosterol in sample to be detected and application
  • Method for separating mannitol, adenosine and ergosterol in sample to be detected and application

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specific Embodiment

[0071] In the first aspect, the present invention proposes a method for separating mannitol, adenosine and ergosterol in edible fungi with matrix solid-phase dispersion extraction technology, and proposes a method for separating adenosine and ergosterol in edible fungi with matrix solid-phase dispersion extraction technology. method of purification. According to a specific embodiment of the present invention, the method includes the following steps:

[0072]Weigh an appropriate amount of dried edible fungus powder, add appropriate amount of diatomaceous earth in a mortar according to the mass ratio of 1:5-1:20 (g / g), grind and mix thoroughly (1-3min), and obtain edible fungus-diatom Soil mixed powder, weigh 0.12-0.4g of the powder for later use. Weigh an appropriate amount of ODS filler (1.0-1.5g), soak it in pure methanol overnight for activation, install it in a small solid-phase extraction column (inner diameter 16mm, column height 80mm, 12mL with a sieve plate), settle, t...

Embodiment 1

[0085] Embodiment 1 Determination of eluent and eluent concentration of eluting impurities and eluting target compound

[0086] Separation and preparation of adenosine and ergosterol based on matrix solid-phase dispersion extraction, comprising the following steps:

[0087] (1) Separation and preparation

[0088] Weigh 0.1 g of fermented Cordyceps powder powder, add 2.0 g of diatomaceous earth into a mortar, grind and mix thoroughly (1 min), to obtain fermented Cordyceps powder-diatomaceous earth (1:20) mixed powder, weigh the Powder 0.4g, put on the solid-phase extraction column (12mL solid-phase extraction column with sieve plate, 1g ODS filler), set up 12 test groups (1-12) respectively, be used for exploring the impurity before eluting adenosine ( Contains mannitol), adenosine, impurities between adenosine and ergosterol, and methanol (ethanol) concentration of ergosterol. Use 9mL a solution, 5mL b solution, 9mL c solution, 9mL d solution to elute impurities and target c...

Embodiment 2

[0100] The optimization of different elution volumes of embodiment 2

[0101] Separation and preparation of adenosine and ergosterol based on matrix solid-phase dispersion extraction, comprising the following steps:

[0102] (1) Separation

[0103] Weigh 0.1g of fermented Cordyceps fungus powder, add 0.5g of diatomaceous earth to the mortar, grind and mix well (1min), get edible fungus-diatomite (1:5) mixed powder, weigh the powder 0.12 g, on a solid-phase extraction cartridge (12mL solid-phase extraction cartridge with sieve plate, 1g ODS filler), and eluted with 9% methanol solution, 30% methanol solution, 96% methanol solution, and 100% methanol solution in sequence , according to polarity, collect one tube per column volume (1.5 mL).

[0104] (2) HPLC detection

[0105] Perform HPLC detection on the eluate from each section and each tube obtained in (1) respectively.

[0106] 9%, 30% methanol eluent detection chromatographic conditions are: chromatographic column (Poro...

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Abstract

The invention provides a method for separating mannitol, adenosine and ergosterol in a sample to be detected. The method comprises the following steps: carrying out elution treatment on a sample to bedetected in a solid-phase extraction column by using a first eluent, a second eluent, a third eluent and a fourth eluent in sequence; and respectively collecting an elution product of the first eluent, an elution product of the second eluent and an elution product of the fourth eluent to obtain an eluent containing mannitol, adenosine and ergosterol successively. The first eluent, the second eluent, the third eluent and the fourth eluent are respectively and independently a methanol aqueous solution, an ethanol aqueous solution, an acetonitrile aqueous solution or any combination of the methanol aqueous solution, the ethanol aqueous solution and the acetonitrile aqueous solution. According to the method, the adenosine and the ergosterol in the sample to be detected can be purified at thesame time, and the purity of the obtained adenosine and the purity of the obtained ergosterol are greatly improved.

Description

technical field [0001] The present invention relates to the field of analysis and detection. Specifically, the present invention relates to methods and applications for separating mannitol, adenosine and ergosterol in samples to be tested. More specifically, the present invention relates to separating mannitol, adenosine and ergot in samples to be tested. A method for sterols and a method for detecting the contents of mannitol, adenosine and ergosterol in a test sample. Background technique [0002] Ergosterol and mannitol are important pharmaceutical and chemical raw materials, widely used in food, medicine and chemical industries. Mannitol is a good diuretic in medicine, reducing intracranial pressure, intraocular pressure and treating kidney medicine, dehydration medicine, sugar substitute, and also used as an excipient for tablets and a diluent for solid and liquid. Adenosine is recognized as an important regulator of neurotransmission and is involved in many physiologi...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/08G01N30/34
CPCG01N30/02G01N30/08G01N30/34G01N2030/062G01N2030/047
Inventor 钱正明吴姿李春红谢美霞李文佳
Owner DONGGUAN HEC CORDYCEPS R&D CO LTD
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