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Composite extraction method for extracting coumarin from radix angelicae dahuricae

A coumarin and extraction technology, applied in the production of bulk chemicals, organic chemistry, etc., can solve the problems of high production cost, difficult industrial application, complex process, etc., to avoid decomposition, low operating temperature, and simple operation process. Effect

Active Publication Date: 2010-10-20
ZHEJIANG UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

The above-mentioned process technologies have their own advantages, but they are difficult to apply industrially due to the problems of complex process and high production cost.

Method used

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  • Composite extraction method for extracting coumarin from radix angelicae dahuricae
  • Composite extraction method for extracting coumarin from radix angelicae dahuricae
  • Composite extraction method for extracting coumarin from radix angelicae dahuricae

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preparation example Construction

[0022] ③ Preparation of reference solution

[0023] Accurately weigh 5.43 mg of imperatorin reference substance and 6.09 mg of isoimperatorin, respectively, and place them in 25 mL volumetric flasks, dilute with methanol to the mark, and shake well. Accurately take 2mL respectively, place in a 10mL volumetric flask, dilute with methanol to the mark, and shake well to obtain a mixed reference solution of imperatorin 43.44 μg / mL and isoimperatorin 48.72 μg / mL.

[0024] ④ Preparation of standard curve:

[0025] Take the above-mentioned mixed reference substance solution, inject samples with different volumes of 5 μL-30 μL according to the chromatographic conditions, take the injection volume (μL) as the abscissa, and the peak area as the ordinate regression, and the equation is: imperatorin y=157.29x- 6.3333 (r=1), the measurement result has a good linear relationship within 0.2172 μg-1.3032 μg; isoimperatorin y=152.52x-30.833 (r=1), the measurement result has a good linear rela...

Embodiment 1

[0031] Take by weighing 1kg and pulverize to 30 orders, the coumarin content is 0.1% the raw material of Angelica dahuricae, put into 5 liters of supercritical extractors. Set the extraction temperature and pressure to 40°C and 30MPa, respectively, and the separation temperature and pressure to 35°C and 5MPa, respectively. 2 After 2 hours of extraction, 5.142 g of extract was obtained. Add 52mL of petroleum ether (boiling range 60-90°C, the same below) at a weight-to-volume ratio of 1:10 to dissolve the extract completely. Then it was extracted twice with 3 times the volume of petroleum ether, and the aqueous layer was discarded. The petroleum ether layer was extracted three times with 60% ethanol at a volume ratio of 1:2.5, the ethanol solution was collected, concentrated under reduced pressure to remove the solvent, and 0.232 g of the product was obtained. Through liquid chromatography analysis, the obtained product contains 39.72% coumarin active ingredients. Among them,...

Embodiment 2

[0033] Weigh 1 kg of Baizhi raw material and crush it to 30 mesh, put it into a 5-liter extractor, the extraction temperature and pressure are 50°C and 25MPa, the separation temperature and pressure are 35°C and 6MPa, respectively, after 2 hours of extraction, 5.156g of extract product. The product was dissolved in 52 mL of petroleum ether, extracted three times with 130 mL of water, and the aqueous phase was discarded. The petroleum ether phase was extracted 4 times with 2.5 volumes of 60% ethanol. The ethanol solvent was collected and concentrated to dryness under reduced pressure to obtain 0.228 g of the product with a total coumarin content of 40.57%. Among them, the content of imperatorin is 24.68%, the content of isoimperatorin is 15.89%

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Abstract

The invention provides a composite extraction method for extracting coumarin from radix angelicae dahuricae. With radix angelicae dahuricae as material and by a method combined with supercritical CO2 extraction and liquid-liquid solvent extraction, the composite extraction method sufficiently utilizes the difference of the dissolving characteristics of the coumarin and impurities in difference solvents to obtain high-purity extract, wherein the content of the coumarin is more than 40 percent. The method overcomes the limitation of the simplex supercritical extraction of the radix angelicae dahuricae, and the operation temperature is low, so that active ingredients can be prevented from being decomposed in the process of extraction. The invention has the advantages of simple operation process, low production cost and easy industrialized application. The obtained extract can be used in the development of medicines, and also can be further refined to obtain various single coumarin compounds.

Description

technical field [0001] The invention belongs to the extraction and processing method of natural products, and mainly relates to a compound extraction method for extracting coumarin from the traditional Chinese medicine Hangbaizhi. Background technique [0002] Hangbaizhi is one of the authentic medicinal materials in Zhejiang, which was first recorded in "Shen Nong's Herbal Classic". Hangbaizhi is warm and pungent in nature, has the effects of dispelling wind and dehumidification, clearing orifices, relieving pain, reducing swelling and discharging pus, and is mainly used clinically to treat colds and headaches, brow bone pain, nasal congestion, toothache, leucorrhea and sore swelling and pain. The main components of Hangbaizhi are volatile oil and coumarin. According to a large number of pharmaceutical experiments, coumarin compounds are the main medicinal components of Hangbaizhi. In recent years, as a large class of natural compounds that are very important in nature, c...

Claims

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Application Information

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IPC IPC(8): C07D493/04C07D311/16
CPCY02P20/54
Inventor 王龙虎梅彦红余立雁刘雪松陈勇
Owner ZHEJIANG UNIV
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