A kind of preparation method of extracting halone from lampstand tree

A technology of lampstand tree and halone, which is applied in the field of preparation of halone, can solve the problems such as the lack of application of high-purity halone industrial production and preparation process reports, etc., to achieve large-scale production operations, less pollution, and less energy consumption Effect

Inactive Publication Date: 2011-12-07
SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In the prior art, there is no report on the preparation process applicable to the industrialized large-scale production of high-purity halone

Method used

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  • A kind of preparation method of extracting halone from lampstand tree

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Effect test

Embodiment 1

[0022] Get 10Kg of light table tree leaves, pulverize, add to CO 2 In the supercritical extractor, methanol is used as an entrainer, the entrainer accounts for 2% by volume of the total extraction solvent, the extraction pressure is 20MPa, the temperature is 40°C, CO 2 The flow rate is 1ml / g crude drug·min, the extraction time is 100min, and the extract is obtained, which is added to a silica gel chromatography column and eluted with a mixed solvent of methanol-chloroform at a ratio of 1:1. The eluate is collected in fractions by column volume and combined. The eluate of the 5th to 8th parts, the solvent was recovered to dryness, and 1.6 g of halone was obtained, which was detected by HPLC with a purity of 95.1%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as CNMR are consistent with the prior art.

Embodiment 2

[0024] Get 10Kg of light table tree leaves, pulverize, add to CO 2 In the supercritical extractor, methanol is used as an entrainer, the entrainer accounts for 4% by volume of the total extraction solvent, the extraction pressure is 30MPa, the temperature is 60°C, CO 2 The flow rate is 3ml / g crude drug min, and the extraction time is 150min. The extract is obtained, added to a silica gel chromatography column, and eluted with a mixed solvent of methanol-chloroform at a ratio of 1:1. The eluate is collected in fractions by column volume and combined. The eluate of the 5th to 8th parts, the solvent was recovered to dryness, and 2.5 g of halone was obtained, which was detected by HPLC with a purity of 94.1%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as CNMR are consistent with the prior art.

Embodiment 3

[0026] Get 10Kg of light table tree leaves, pulverize, add to CO 2 In the supercritical extractor, methanol is used as an entrainer, the entrainer accounts for 3% by volume of the total extraction solvent, the extraction pressure is 25MPa, the temperature is 50°C, CO 2 The flow rate is 2ml / g crude drug min, and the extraction time is 120min. The extract is obtained, added to a silica gel chromatography column, and eluted with a methanol-chloroform mixed solvent with a ratio of 1:1. The eluate is collected in fractions by column volume and combined. The eluate of the 5th to 8th parts, the solvent was recovered to dryness, and 2.1 g of halone was obtained, which was detected by HPLC with a purity of 96.8%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as CNMR are consistent with the prior art.

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Abstract

The present invention relates to a preparation method for extracting halone from lampstand tree with simple operation, less pollution and less energy consumption. agent, to obtain the extract, added to a silica gel chromatography column, and eluted with a methanol-chloroform mixed solvent with a ratio of 1:1, and the eluent was collected in fractions by column volume, and the eluents of the 5th to 8th parts were combined, Recover the solvent to dryness, that is, too. By adopting the invention to prepare the halone, the product has high purity and is easy to realize industrial scale-up.

Description

technical field [0001] The invention relates to a method for preparing halone, in particular to a method for extracting halone from plants. Background technique [0002] Rengyolone, molecular formula: C 8 h 10 o 3 , Molecular weight: 154.165, CAS registration number: 93675-87-7, mainly exists in various plants of Cornaceae, Labiatae, Scrophulariaceae, among which the plant of Cornaceae Bothrocaryum controversum Rich in Hemsl. Its molecular formula is as follows. [0003] [0004] Modern studies have shown that halone has anti-tumor effects, and it is also used as a raw material for the synthesis of other active derivatives. [0005] Dogwood lighthouse tree Bothrocaryum controversum The leaves of Hemsl. are used as a traditional Chinese medicine, which can clear away heat and calm the liver, reduce swelling and relieve pain. [0006] In the prior art, there is no report on the preparation process applicable to the industrialized large-scale production of high-puri...

Claims

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Application Information

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IPC IPC(8): C07D307/83
CPCY02P20/54
Inventor 王峰王琳张发成
Owner SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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