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Method for extracting 7-beta-hydroxyl cholesterol from osteon myospalacem baileyi

A technology of hydroxycholesterol and sialon bone, applied in the direction of steroids, organic chemistry, etc., can solve the problems that hinder the progress of 7-β-hydroxycholesterol, and achieve the effect of improving efficiency, compound purity, peak capacity, and high consistency

Inactive Publication Date: 2015-01-14
ZHENGYUANTANG TIANJIN BINHAI NEW AREA BIOTECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] But so far, the method of extracting 7-β-hydroxycholesterol from natural product extracts has not been reported, let alone extracting high-purity or monomeric 7-β-hydroxycholesterol, which also hinders to a certain extent. The progress of 7-β-hydroxycholesterol in the development of animal medicine as traditional Chinese medicine

Method used

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  • Method for extracting 7-beta-hydroxyl cholesterol from osteon myospalacem baileyi
  • Method for extracting 7-beta-hydroxyl cholesterol from osteon myospalacem baileyi
  • Method for extracting 7-beta-hydroxyl cholesterol from osteon myospalacem baileyi

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Embodiment 1

[0024] Take the Theron bone as the raw material, grind it into powder, weigh 2.5g, dissolve it in 50mL of 1% ethanol-n-hexane solution, and prepare the Theron bone extract solution with a concentration of 50mg / mL, and pass through a 0.45μm microporous membrane , for one-dimensional liquid chromatography preparation. One-dimensional liquid chromatography adopts DAISO Silica150×250mm, 10μm, The mobile phase is a mixture of organic phases, in which the organic phase A is n-hexane, B is ethanol, and the isocratic elution method: B phase concentration is 1% isocratic for 12 minutes, 5% isocratic for 10 minutes, 8% etc. 10 minutes isocratic at 15%, 10 minutes isocratic at 15%, 25 minutes isocratic at 30%, 15 minutes isocratic at 50%, 15 minutes isocratic at 70%, 15 minutes isocratic at 100%. Use an ultraviolet detector at 214nm to select the absorption wavelength, the preparation temperature is room temperature, the injection volume is 5000 μL / needle, the flow rate of the mobile p...

Embodiment 2

[0026] Take the Theron bone as the raw material, grind it into powder and weigh 5g, dissolve it in 50mL of 5% ethanol-n-hexane solution to prepare the Theron bone extract solution with a concentration of 100mg / mL, pass through a 0.45μm microporous membrane, Perform one-dimensional liquid chromatography preparatively. One-dimensional liquid chromatography adopts DAISO Silica150×250mm, 10μm, The mobile phase is a mixture of organic phases, in which the organic phase A is n-hexane, B is ethanol, isocratic elution method: B phase concentration is 1% isocratic for 12 minutes, 5% isocratic for 10 minutes, 8% etc. 10 minutes isocratic at 15%, 10 minutes isocratic at 15%, 25 minutes isocratic at 30%, 15 minutes isocratic at 50%, 15 minutes isocratic at 70%, 15 minutes isocratic at 100%. The absorption wavelength was selected by an ultraviolet detector at 214 nm, the preparation temperature was room temperature, the injection volume was 5000 μL / needle, the mobile phase flow rate was ...

Embodiment 3

[0028]Take Theron bone as raw material, grind it into powder, weigh 2.5g, dissolve it in 100mL of 5% ethanol-n-hexane solution, and prepare the Theron bone extract solution with a concentration of 25mg / mL, and pass through a 0.45μm microporous membrane , for one-dimensional liquid chromatography preparation. One-dimensional liquid chromatography adopts DAISO Silica150×250mm, 10μm, The mobile phase is a mixture of organic phases, in which the organic phase A is n-hexane, B is ethanol, isocratic elution method: B phase concentration is 1% isocratic for 12 minutes, 5% isocratic for 10 minutes, 8% etc. 10 minutes isocratic at 15%, 10 minutes isocratic at 15%, 25 minutes isocratic at 30%, 15 minutes isocratic at 50%, 15 minutes isocratic at 70%, 15 minutes isocratic at 100%. Use an ultraviolet detector at 214nm to select the absorption wavelength, the preparation temperature is room temperature, the injection volume is 5000 μL / needle, the flow rate of the mobile phase is 80mL / min...

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Abstract

The invention provides a method for extracting 7-beta-hydroxyl cholesterol from osteon myospalacem baileyi. The method comprises the following steps: dissolving osteon myospalacem baileyi to 50-200mg / mL by using 1-15% ethanol-normal hexane; carrying out one-dimensional liquid chromatography, wherein the phase A is normal hexane and the phase B is ethanol, and the eluting mode is as follows: for the phase B: 1% isocratic elution for 12 minutes, 5% isocratic elution for 10 minutes, 8% isocratic elution for 10 minutes, 15% isocratic elution for 10 minutes, 30% isocratic elution for 25 minutes, 50% isocratic elution for 15 minutes, 70% isocratic elution for 15 minutes and 100% isocratic elution for 15 minutes; collecting a target component according to ultraviolet absorption spectrums; dissolving to 50-100mg / mL by using 2-15% ethanol-normal hexane; carrying out two-dimensional liquid chromatography, wherein the phase A is normal hexane and the phase B is ethanol, and the eluting mode is as follows: for the phase B: 5% isocratic elution for 30 minutes; and collecting a target component according to ultraviolet absorption spectrums to obtain the target extract. The purity of 7-beta-hydroxyl cholesterol obtained by the method is over 99%.

Description

technical field [0001] The invention relates to the technical field of medical products, in particular to a method for extracting high-purity 7-beta-hydroxycholesterol from Theron bone. Background technique [0002] Steroids are widely distributed in traditional Chinese medicine animal medicines, and their chemical structures are complex and diverse, and their biological activities are remarkable. Some animal steroids with novel structures have remarkable physiological and pharmacological activities, and may be an important source of drugs for the treatment of a series of major human diseases. 7-β-hydroxycholesterol is such a steroidal compound, which is an important natural active ingredient widely present in animals, and its structure is as follows: [0003] [0004] At present, it has been found that the activities of 7-β-hydroxycholesterol mainly include the following points: first, it can inhibit the proliferation, differentiation and cytotoxicity of proliferating a...

Claims

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Application Information

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IPC IPC(8): C07J9/00
CPCC07J9/00
Inventor 张耀洲江磊陶雁铎王丹
Owner ZHENGYUANTANG TIANJIN BINHAI NEW AREA BIOTECH
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