Preparation method of fraxinellone, dictamnine and obakunone

A technology of white fresh alkali and phellodendron, applied in the field of natural medicine, can solve the problems that the components cannot be fully extracted, the production efficiency cannot be satisfied, the yield cannot meet the production requirements, etc., and the cost is low, the process is controllable, and the operation simple effect

Pending Publication Date: 2018-10-23
成都瑞芬思德丹生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the prior art, the yields of extracting arketone, dichroicine, and phellodendron from the white fresh bark cannot meet the production requirements, and these three components cannot be fully extracted, and cannot meet the needs of production efficiency.

Method used

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  • Preparation method of fraxinellone, dictamnine and obakunone
  • Preparation method of fraxinellone, dictamnine and obakunone
  • Preparation method of fraxinellone, dictamnine and obakunone

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preparation example Construction

[0024] The present invention provides a kind of preparation method of arketone, cylindrine and cortex ketone, comprising the following steps:

[0025] 1) Provide white fresh bark or white willow bark medicinal material, extract with 50%-90% alcohol solution, preferably 70%-80% alcohol solution, more preferably ethanol or methanol solution, combine extract A, concentrate under reduced pressure Concentrate B was obtained. The extraction method is one or more of reflux extraction, percolation extraction and ultrasonic extraction. Reflux extraction or percolation extraction is preferred. The volume-to-weight (L / kg) ratio of the solvent for reflux extraction to medicinal materials is (2-5):1, the extraction temperature for reflux extraction is 50°C-70°C, the extraction time is 1-2h, and the extraction times are 4-6 times.

[0026] 2) The concentrated solution B was extracted with ethyl acetate, the ethyl acetate layers were combined, and concentrated under reduced pressure to obt...

Embodiment 1

[0035] 1. Extraction

[0036] Take white fresh bark medicinal materials or white willow bark medicinal materials, grind them, and extract them with organic solvents such as methanol, ethanol, ethyl acetate, dichloromethane, etc., the extraction method is reflux extraction, the ratio of feeding liquid to material is 3:1, and the extraction temperature is 60°C , extracted 1.5 hours each time, extracted 5 times, combined all the extracts A, concentrated under reduced pressure at 50-70 ° C, concentrated to no alcohol, collected the concentrate B, and set aside.

[0037] 2. Extraction pretreatment

[0038] The extraction concentrate B collected in the previous step is extracted by adding ethyl acetate at a volume ratio of 1:1, extracting 3-5 times, collecting and combining the ethyl acetate layers, concentrating under reduced pressure at 50-70°C, and concentrating to extract C ,spare.

[0039] 3. Separation and purification:

[0040] Separation and purification method: silica ge...

Embodiment 2

[0050] 1. Extraction

[0051] Take white fresh bark medicinal material or white willow bark medicinal material, pulverize, and extract with concentration of 50% ethanol, 60% ethanol, 75% ethanol, 80% ethanol, 90% ethanol, the extraction method is reflux extraction, and the ratio of feeding liquid to material is 3: 1. Extraction temperature is 70°C, extraction time is 1h, extract 4 times, combine all extracts A, concentrate under reduced pressure at 50-70°C, concentrate until alcohol-free, collect concentrate B, set aside.

[0052] 2. Extraction pretreatment

[0053] The extraction concentrate B collected in the previous step is extracted by adding ethyl acetate at a volume ratio of 1:1, extracting 3-5 times, collecting and combining the ethyl acetate layers, concentrating under reduced pressure at 50-70°C, and concentrating to extract C ,spare.

[0054] 3. Separation and purification:

[0055] Separation and purification method: silica gel chromatography

[0056] Purificat...

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Abstract

The invention discloses a preparation method of fraxinellone, dictamnine and obakunone, which includes steps of: 1) preparing cortex dictamni or white willow bark medicine materials, extracting the materials with a 50-90% alcohol solution, mixing extracts A, and performing pressure reduced concentration to obtain a concentrate B; 2) extracting the concentrate B with ethyl acetate and performing pressure reduced concentration to obtain a concrete C; 3) performing chromatographic separation to the concrete C, performing gradient elution with a petroleum ether-ethyl acetate system, collecting a solution D when volume ratio of the petroleum ether to ethyl acetate ranges from 50:1 to 30:1, collecting a solution E when volume ratio of the petroleum ether to ethyl acetate ranges from 30:1 to 15:1, and collecting a solution F when volume ratio of the petroleum ether to ethyl acetate ranges from 15:1 to 2:1; 4) concentrating the solutions into concretes, and recrystallizing and drying the concretes to prepare pure products of the fraxinellone, dictamnine and obakunone. The method can reach 90% in yield and higher than 99% in purity, and is suitable for industrial production.

Description

technical field [0001] The invention relates to the field of natural medicinal chemicals, in particular to a preparation method of arketone, whitewashine and cortex ketone. Background technique [0002] The traditional Chinese medicine Dictamnus dasycarpus Turcz is the dried root bark of Dictamnus dasycarpus Turcz, which has the functions of expelling wind, dampness, heat and detoxification. Modern pharmacological studies have shown that Cortex radix has various activities such as anti-oxidation, anti-virus, anti-bacteria, anti-inflammation, and anti-tumor. Studies in recent years have shown that the main medicinal components of D. japonicus are the alkone, dichroicine, and phellodendron isolated from D. japonicus, which have a variety of strong biological activities. However, in the prior art, the yields of extracting arketone, leuconine and phellodendron from the white fresh bark cannot meet the production requirements, these three components cannot be fully extracted, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/10C07D491/048C07D307/88
CPCC07D307/88C07D491/048C07D493/10
Inventor 董维珍常建红寇俊闯
Owner 成都瑞芬思德丹生物科技有限公司
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