Preparation method of griseofulvin

Abstract

The invention discloses a preparation method of griseofulvin. The preparation method comprises the following steps of: A, heating griseofulvin fermentation liquor, adding calcium oxide to adjust the PH, carrying out solid-liquid separation by using a sheet frame, adding calcium oxide to a filter cake to granulate, and extracting by using acetone to obtain a griseofulvin acetone extracting solution; B, decoloring the griseofulvin acetone extracting solution by using an active carbon column to obtain a griseofulvin decoloring solution, feeding the decoloring solution into a concentration tank, and crystallizing by concentrating to obtain wet griseofulvin crystals; and C, washing the wet griseofulvin crystals once by using a dichloromethane and ethanol mixed solution while stirring, then washing the wet griseofulvin crystals once by using medicinal ethanol with the concentration of 95 percent while stirring, drying the crystals by using a vacuum drier, and carrying out superfine grinding on the dried crystals to obtain the griseofulvin product. Compared with a traditional preparation method, the preparation method disclosed by the invention has the advantages that the crystallization times in the process of preparing the griseofulvin in the prior art is reduced, the yield loss caused by recrystalization of griseofulvin is effectively avoided, the total yield of the griseofulvin is improved by 7-10 percent, and the production cost is greatly reduced.

Description

technical field

[0001] The invention relates to a preparation method of a raw material drug, in particular to a preparation method of griseofulvin. Background technique

[0002] Griseofulvin is an antibiotic raw material drug. Its English name is Griseofulvin. Its Chinese aliases are griseofulvin and microcrystalline griseofulvin. 07-8, this product is white or off-white fine powder; this product mainly has good antibacterial effect on superficial fungi such as Trichophyton, Microsporum, and Epidermophyton.

[0003] Griseofulvin is indicated for the treatment of various tinea conditions, including tinea capitis, tinea barbae, tinea corporis, jock itch, tinea pedis and onychomycosis.

[0004] At present, the method for preparing griseofulvin generally comprises the following steps: a: heating with griseofulvin fermented liquid, solid-liquid separation in plates and frames, filter cake granulation, acetone extraction to obtain griseofulvin acetone extract; b, The griseofulvi...

Examples

Embodiment 1

[0013] Example 1 A preparation method of griseofulvin, comprising the following steps:

[0014] A. Heating the griseofulvin fermentation broth to 80°C, adding calcium oxide to adjust the pH to 5.5, separating solid-liquid from the plate and frame, adding calcium oxide to the filter cake for granulation, and acetone extraction to obtain griseofulvin acetone extract;

[0015] B, the griseofulvin acetone extract is decolorized by the activated carbon column to obtain the griseofulvin acetone decolorization solution, and the decolorized solution enters the concentration tank, and decompresses by the way of steam circulating heating in the jacket and vacuuming of the tank to reduce the boiling point of acetone Concentrated, the concentration temperature is controlled at 27 o C, the vacuum degree is controlled at -0.09MPa, after concentration, the acetone evaporates rapidly, is cooled and recovered, recycled, and the crystals are naturally separated out. Under vacuum conditions, ...

Embodiment 2

[0018] Example 2 A preparation method of griseofulvin, comprising the following steps:

[0019] A. Heating the griseofulvin fermentation broth to 100°C, adding calcium oxide to adjust the pH to 6, separating solid-liquid from the plate and frame, adding calcium oxide to the filter cake for granulation, and acetone extraction to obtain griseofulvin acetone extract;

[0020] B, the griseofulvin acetone extract is decolorized by the activated carbon column to obtain the griseofulvin acetone decolorization solution, and the decolorized solution enters the concentration tank, and decompresses by the way of steam circulating heating in the jacket and vacuuming of the tank to reduce the boiling point of acetone Concentrated, the concentration temperature is controlled at 24 o C, the vacuum degree is controlled at -0.07MPa, after concentration, the acetone evaporates rapidly, is cooled and recovered, recycled, and the crystals are naturally precipitated. When the acetone is not comp...

Embodiment 3

[0023] Example 3 A preparation method of griseofulvin, comprising the following steps:

[0024] A. The griseofulvin fermentation broth is heated to 90°C, calcium oxide is added to adjust the pH to 6.5, solid-liquid separation of the plate and frame, granulation of the filter cake with calcium oxide, and acetone extraction to obtain the griseofulvin acetone extract;

[0025] B, the griseofulvin acetone extract is decolorized by the activated carbon column to obtain the griseofulvin acetone decolorization solution, and the decolorized solution enters the concentration tank, and decompresses by the way of steam circulating heating in the jacket and vacuuming of the tank to reduce the boiling point of acetone Concentrated, the concentration temperature is controlled at 30 o C, the vacuum degree is controlled at -0.08MPa, after concentration, the acetone evaporates rapidly, is cooled and recovered, recycled, and the crystals are naturally separated out. Under vacuum conditi...

technical field

[0001] The invention relates to a preparation method of a raw material drug, in particular to a preparation method of griseofulvin. Background technique

[0002] Griseofulvin is an antibiotic raw material drug. Its English name is Griseofulvin. Its Chinese aliases are griseofulvin and microcrystalline griseofulvin. 07-8, this product is white or off-white fine powder; this product mainly has good antibacterial effect on superficial fungi such as Trichophyton, Microsporum, and Epidermophyton.

[0003] Griseofulvin is indicated for the treatment of various tinea conditions, including tinea capitis, tinea barbae, tinea corporis, jock itch, tinea pedis and onychomycosis.

[0004] At present, the method for preparing griseofulvin generally comprises the following steps: a: heating with griseofulvin fermented liquid, solid-liquid separation in plates and frames, filter cake granulation, acetone extraction to obtain griseofulvin acetone extract; b, The griseofulvi...

Examples

Embodiment 1

[0013] Example 1 A preparation method of griseofulvin, comprising the following steps:

[0014] A. Heating the griseofulvin fermentation broth to 80°C, adding calcium oxide to adjust the pH to 5.5, separating solid-liquid from the plate and frame, adding calcium oxide to the filter cake for granulation, and acetone extraction to obtain griseofulvin acetone extract;

[0015] B, the griseofulvin acetone extract is decolorized by the activated carbon column to obtain the griseofulvin acetone decolorization solution, and the decolorized solution enters the concentration tank, and decompresses by the way of steam circulating heating in the jacket and vacuuming of the tank to reduce the boiling point of acetone Concentrated, the concentration temperature is controlled at 27 o C, the vacuum degree is controlled at -0.09MPa, after concentration, the acetone evaporates rapidly, is cooled and recovered, recycled, and the crystals are naturally separated out. Under vacuum conditions, ...

Embodiment 2

[0018] Example 2 A preparation method of griseofulvin, comprising the following steps:

[0019] A. Heating the griseofulvin fermentation broth to 100°C, adding calcium oxide to adjust the pH to 6, separating solid-liquid from the plate and frame, adding calcium oxide to the filter cake for granulation, and acetone extraction to obtain griseofulvin acetone extract;

[0020] B, the griseofulvin acetone extract is decolorized by the activated carbon column to obtain the griseofulvin acetone decolorization solution, and the decolorized solution enters the concentration tank, and decompresses by the way of steam circulating heating in the jacket and vacuuming of the tank to reduce the boiling point of acetone Concentrated, the concentration temperature is controlled at 24 o C, the vacuum degree is controlled at -0.07MPa, after concentration, the acetone evaporates rapidly, is cooled and recovered, recycled, and the crystals are naturally precipitated. When the acetone is not comp...

Embodiment 3

[0023] Example 3 A preparation method of griseofulvin, comprising the following steps:

[0024] A. The griseofulvin fermentation broth is heated to 90°C, calcium oxide is added to adjust the pH to 6.5, solid-liquid separation of the plate and frame, granulation of the filter cake with calcium oxide, and acetone extraction to obtain the griseofulvin acetone extract;

[0025] B, the griseofulvin acetone extract is decolorized by the activated carbon column to obtain the griseofulvin acetone decolorization solution, and the decolorized solution enters the concentration tank, and decompresses by the way of steam circulating heating in the jacket and vacuuming of the tank to reduce the boiling point of acetone Concentrated, the concentration temperature is controlled at 30 o C, the vacuum degree is controlled at -0.08MPa, after concentration, the acetone evaporates rapidly, is cooled and recovered, recycled, and the crystals are naturally separated out. Under vacuum conditi...