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Extraction method of silibinin

A technology of silibinin and extraction method, which is applied in the field of silibinin extraction, can solve the problems such as the lack of silybin extraction method, and achieve the effect of improving related substances, good effect and high product purity

Inactive Publication Date: 2018-03-13
江苏健佳药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there is a lack of an extraction method for silibinin without harmful and toxic solvent residues

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A method for extracting silybin of the present invention comprises the following steps: (1) cleaning the silymarin shell to be extracted, draining the water, and then performing microwave drying to reduce the water content to below 10%; The temperature is 50°C. The microwave drying frequency is 1000 MHz, and the drying time is 6 min.

[0027] (2) adding ethyl acetate to dissolve the milk thistle shell, extracting the total flavonoids, and collecting ketones in a vacuum; the mass ratio of the milk thistle shell to the ethyl acetate is 1:3.5.

[0028] (3) After the total flavonoids are dissolved in water, the precipitate obtained is added to an ethanol solution to dissolve the crude product of silibinin. Using acetone as a solvent, the crude product of silibinin is added for heating and dissolving, and heated to reflux, wherein acetone and silybin The mass ratio of crude product is 16:1;

[0029] (4) adopt macroporous cation exchange resin to adsorb, thereby obtain satu...

Embodiment 2

[0033] The difference between embodiment 2 and embodiment 1 is:

[0034] A method for extracting silybin of the present invention comprises the following steps: in step (1), drain the water after cleaning the silymarin shell to be extracted, and then carry out microwave drying to reduce the water content to 10 % or less; the extraction temperature is 65°C. The microwave drying frequency is 800 MHz, and the drying time is 5 min.

[0035] In step (2), ethyl acetate is added to dissolve the milk thistle shell, the total flavonoids are extracted, and the ketone is collected in a vacuum; the mass ratio of the milk thistle shell to the ethyl acetate is 1:4.

[0036] In step (3), after the total flavonoids are dissolved in water, the precipitate is added to ethanol solution to dissolve the crude product of silibinin, using acetone as the solvent, adding the crude product of silybin for heating and dissolving, and heating to reflux, wherein the acetone and The mass ratio of crude si...

Embodiment 3

[0040] The difference between embodiment 3 and embodiment 1 is:

[0041] A method for extracting silybin of the present invention comprises the following steps: in step (1), drain the water after cleaning the silymarin shell to be extracted, and then carry out microwave drying to reduce the water content to 10 % or less; the extraction temperature is 85°C. The microwave drying frequency is 900 MHz, and the drying time is 4 minutes.

[0042] In step (2), ethyl acetate is added to dissolve the milk thistle shell, the total flavonoids are extracted, and the ketone is collected in a vacuum; the mass ratio of the milk thistle shell to the ethyl acetate is 1:3.8.

[0043] In step (3), after the total flavonoids are dissolved in water, the precipitate is added to ethanol solution to dissolve the crude product of silibinin, using acetone as the solvent, adding the crude product of silybin for heating and dissolving, and heating to reflux, wherein the acetone and The mass ratio of si...

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Abstract

The invention discloses an extraction method of silibinin. The extraction method includes following steps: (1), washing silibinin to be extracted, draining water, and performing microwave drying to enable moisture in silibinin to be lowered to below 10%; (2), adding ethyl acetate to dissolve silibinin, extracting total flavone, and collecting ketone in vacuum; (3), adding water to dissolve total flavones to obtain precipitate, adding alcohol solution for dissolving to obtain a silibinin coarse product, adopting acetone as a solvent, adding the silibinin coarse product, heating for dissolving,and heating till backflow; (4), performing acid pickling on saturated macroporous resin and alcohol washing sequentially to obtain alcohol solution of silibinin; (5), cooling and stirring for crystallization, stirring, filtering, washing with 95% alcohol, draining, and drying a filter cake to obtain a silibinin finished product; (6), performing secondary vacuum drying and concentrating to obtain refined silibinin. The extraction method is simple, efficient, free of harmful and toxic solvent residue, high in product purity, environment-friendly and suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of silybin, in particular to a method for extracting silybin. Background technique [0002] Milk thistle (Silybum marianum (L.) Gaertn) is a plant of the genus Silybum in the family Asteraceae. It is an excellent medicinal plant and oil plant. The dried ripe fruit is used as medicine. It tastes bitter and cool, and returns to the liver and gall bladder. , has the functions of clearing heat and detoxifying, soothing the liver and promoting gallbladder, and is used to treat damp-heat in the liver and gallbladder, hypochondriac pain, and jaundice. [0003] Milk thistle is native to Europe, the Mediterranean region, North Africa and central Asia. In 1952, the Beijing Botanical Garden introduced it from the United Kingdom as an ornamental plant, and in 1972, it was introduced from Germany by the Tianjin Native Products Branch of China Native Products and Animal Products Import and Export Corporation as a medicin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D407/04
CPCC07D407/04
Inventor 周勇周晓娟梁呈元
Owner 江苏健佳药业有限公司
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