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A kind of method for preparing muscone

A technology of musk ketone and musk, which is applied in the pharmaceutical field, can solve the problems of low purity, poor extraction effect, loss and the like, and achieves the effects of high purity, good extraction effect and mild processing conditions

Active Publication Date: 2018-09-14
安徽瑞邦香料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process of extracting muscone from musk is too simple, and the extraction effect is poor, and the purity is low, causing certain losses

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] In an embodiment of the present invention, a method for preparing muscone comprises the following steps:

[0025] 1) Crush musk, pass through a 60-mesh sieve, soak in 75v% ethanol at 40°C for 3 hours, then reflux and extract with 8 times the weight of 75v% ethanol for 3 times, reflux for 3 hours each time, filter, and take the filter residue and filtrate for later use.

[0026] 2) The filter residue was reflux extracted twice with 8 times the weight of water, each extraction was 3h, filtered, the filter residue was collected, and the filtrate was combined with the filtrate in step 1) for later use.

[0027] 3) Soak the filter residue in step 2) with hot water at 50°C for 4 hours, and then use 6 times the mass of water for injection for hot-press distillation extraction for 4 hours. Hot-press extraction needs to control the pressure of the container at 0.3MPa and the temperature at 90°C. Prepare hot-pressed extract.

[0028] 4) Combine the hot-pressed extract with the c...

Embodiment 2

[0034] In an embodiment of the present invention, a method for preparing muscone comprises the following steps:

[0035] 1) Crush musk, pass through a 100-mesh sieve, soak in 95v% ethanol at 50°C for 5 hours, then reflux extract with 15 times the weight of 95v% ethanol for 4 times, reflux for 4 hours each time, filter, and take the filter residue and filtrate for later use.

[0036] 2) The filter residue was reflux extracted with 15 times the weight of water for 3 times, each time for 4 hours, filtered, and the filter residue was collected, and the filtrate was combined with the filtrate in step 1) for later use.

[0037] 3) Soak the filter residue in step 2) with hot water at 55°C for 8 hours, and then use 9 times the mass of water for injection to extract by hot-press distillation for 6 hours. The pressure of the hot-press extraction needs to be controlled at 0.5 MPa and the temperature at 125°C. Prepare hot-pressed extract.

[0038] 4) Combine the hot-pressed extract with ...

Embodiment 3

[0044] 1) Crush musk, pass through a 80-mesh sieve, soak in 95v% ethanol at 45°C for 4 hours, then reflux and extract with 12 times the weight of 95v% ethanol for 3 times, each time for 3.5h, filter, and take the filter residue and filtrate for later use.

[0045] 2) Refluxing the filter residue with 12 times the weight of water and extracting twice for 3.5 hours each time, filtering, collecting the filter residue, and combining the filtrate with the filtrate in step 1) for later use.

[0046] 3) Soak the filter residue in step 2) with hot water at 52°C for 6 hours, and then use 7.5 times the mass of water for injection for hot-press distillation extraction for 5 hours. The hot-press extraction needs to control the pressure of the container at 0.4MPa and the temperature at 110°C. Prepare hot-pressed extract.

[0047] 4) Combine the hot-pressed extract with the combined filtrate in step 2), concentrate to an extract with a relative density of 1.2 at 60°C, add ethanol, and centr...

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PUM

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Abstract

The invention discloses a method for preparing musk ketone efficiently and mildly. The method comprises the following steps: crushing musk, sieving musk, soaking musk by using ethanol, performing reflux extraction by using ethanol, and performing reflux extraction by using water to obtain a filtrate; soaking a filter residue by using hot water, and performing hot-pressing distillation extraction to obtain a hot-pressed extract; concentrating the hot-pressed extract and the filtrate, centrifuging, washing, and dissolving in distilled water to obtain a dissolved solution; adjusting the pH of the dissolved solution, filtering by using a ceramic membrane, circularly washing, adding pure water for dissolving, decolorizing, filtering, and performing spray drying to obtain the musk ketone. By the method, the purity of the musk ketone can be increased, and reaches above 99%; the preparation process is simple, and easy to operate; a treatment condition is mild, so that the musk ketone is not affected; the extracting effect is good, more than 99% of the musk ketone in the musk can be extracted; the method has the advantages of high efficiency, rapidness, achievement of high purity, and the like.

Description

technical field [0001] The invention relates to the technical field of pharmacy, in particular to a method for preparing muscone. Background technique [0002] Musk is made from the dried secretion of the male gland sac of deer musk deer. It is a high-grade spice. If you put a little in the room, it will fill the room with a delicate fragrance and a very different smell. Musk is not only fragrant and pleasant, but also has a long-lasting fragrance. Musk has been used in China for a long time. Du Fu, a poet of the Tang Dynasty, met in the poem "Lilac": "Falling into the orchid musk at night". Musk is an important raw material for the preparation of high-end essence. Ancient literati, poets, and painters all added a little musk to the finest musk material to make "musk ink" for writing and painting, which is fragrant and quiet. Musk is warm in nature, non-toxic, bitter in the mouth. Go into the heart, spleen, liver meridian, have one's ideas straightened out, ward off dir...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/78C07C49/385
CPCC07C45/78C07C49/385
Inventor 韩朝金马飞栾志华
Owner 安徽瑞邦香料有限公司
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