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Method for extracting and separating cucurbitacin B

A separation method, cucurbitacin technology, applied in the direction of steroids, organic chemistry, etc., to achieve the effect of improving the extraction rate, simple production process, and easy operation

Active Publication Date: 2010-06-30
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are many studies on the synthesis of natural products and the structural modification of lead compounds using the structural transformation method, but there are few reports on the extraction and separation of active components of natural products, and it is used as an extraction method or technology. The application of the concept to extraction and separation has not yet been reported

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: the preparation of total cucurbitacin extract

[0024] 1 kg of raw melon pedicles was crushed, and refluxed with 95% ethanol at 80°C for 3 times, each time for 1 hour. After the extract was concentrated, it was extracted three times with 3-4 times the volume of ethyl acetate, and the ethyl acetate extract was extracted Concentrate again, get total cucurbitacin extract 138.6g.

Embodiment 2

[0026] Take 0.58g of total cucurbitacin extract, add 50ml of 0.1mol / L acetic acid (prepared with 30% volume fraction ethanol aqueous solution), heat and reflux in a water bath at 80°C for 2 hours, adjust the pH to 7 after the reflux, and concentrate to dryness under reduced pressure. Then dilute to 100ml with methanol. The sample was detected by HPLC, and the content of cucurbitacin B in the total cucurbitacin extract was measured to be 60.39 mg.

[0027] The same method was used to do a control test. Take 0.58g of total cucurbitacin extract, add 50ml of ethanol aqueous solution with a volume fraction of 30%, heat and reflux for 2h in a water bath at 80°C, adjust the pH to 7 after the reflux, concentrate to dryness under reduced pressure, and then use methanol Dilute to 100ml. The sample was detected by HPLC, and the content of cucurbitacin B in the total cucurbitacin extract was measured to be 54.63 mg.

Embodiment 3

[0029] Take 0.5g of total cucurbitacin extract, add 50ml of 0.2mol / L acetic acid (prepared with 30% volume fraction ethanol aqueous solution), heat and reflux in a water bath at 80°C for 2 hours, adjust the pH to 7 after the reflux, and concentrate to dryness under reduced pressure. Then dilute to 100ml with methanol. The sample was detected by HPLC, and the content of cucurbitacin B in the total cucurbitacin extract was measured to be 57.53 mg.

[0030] The same method was used to do a control test. Take 0.58g of total cucurbitacin extract, add 50ml of ethanol aqueous solution with a volume fraction of 30%, heat and reflux for 2h in a water bath at 80°C, adjust the pH to 7 after the reflux, concentrate to dryness under reduced pressure, and then use methanol Dilute to 100ml. The sample was detected by HPLC, and the content of cucurbitacin B in the total cucurbitacin extract was measured to be 54.63 mg.

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Abstract

The invention discloses a method for extracting and separating cucurbitacin B, which comprises the following steps: firstly, melon pedicels as a raw material are crushed and are refluxed and extracted by ethanol diacolation or ethanol, an extracting solution is extracted by ethyl acetate more than three times after being concentrated, and the ethyl acetate is recovered to obtain a total cucurbitacin extract; secondly, the total cucurbitacin extract is taken to be dissolved in a 25 to 45 percent of ethanol water solution, and the hydrolysis reaction is carried out in the presence of acetic acid; the pH value is adjusted to be neutral after full reaction, and the extract is concentrated to dry; and then the obtained extract is treated by purification so as to obtain a cucurbitacin B product with more than 60 percent of cucurbitacin B content, and the concentration of the acetic acid is 0.1 to 0.3 mol / L. Compared with the prior art for extracting and separating cucurbitacin B, the invention has the following advantages: the analogue (such as cucurbitacin B glucoside) of the cucurbitacin B is converted into the cucurbitacin B by the structural transformation in the process of extraction, so that the extraction rate of the cucurbitacin B is improved, the production process is simple, and the operation is simple.

Description

technical field [0001] The invention relates to the extraction and separation of active ingredients of natural products, in particular to a method for the extraction and separation of cucurbitacin B. Background technique [0002] Cucurbitacin B is a cucurbitane substance distributed in a variety of plants. People have found the distribution of cucurbitacin B in muskmelon, gourd, Baixie root and other plants. However, the traditional cucurbitacin B extraction techniques mainly include: ethanol thermal extraction method, ultrasonic ethanol extraction method, etc. In these extraction and separation methods and technologies, the technical principles are based on the physical and chemical properties of target compounds with biological activity. The corresponding separation method and technology is a physical process in the whole process, which does not consider the comprehensive utilization of all chemical components of natural products, so the resource utilization rate is low, t...

Claims

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Application Information

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IPC IPC(8): C07J9/00
Inventor 单伟光唐岚单海峰占扎君
Owner ZHEJIANG UNIV OF TECH
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