Method for extracting bergapten from radix angelicae pubescentis

A technology of bergamot lactone and lodo, which is applied in the field of extraction and purification of bergamot lactone, can solve problems such as poor extraction effect, and achieve the effects of saving labor intensity, increasing content, and avoiding losses

Inactive Publication Date: 2010-08-18
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In recent years, high-performance liquid chromatography has also been widely used to separate co

Method used

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  • Method for extracting bergapten from radix angelicae pubescentis

Examples

Experimental program
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Effect test

Example Embodiment

[0024] Example 1:

[0025] Pulverize it to 60 meshes, take 10kg (bergamot lactone content 0.0046%) and add 100L 70% ethanol for reflux extraction for 3 hours, filter to obtain 104L extract, add 50g activated carbon, stir and decolorize at 40℃, pump the decolorizing solution into the pretreated Silica medium pressure column, elute with 9:1 petroleum ether / ethyl acetate mixture at a flow rate of 60ml / min, collect eluent at 500ml each, identify each component by TLC, and combine the bergamot lactone-containing segment to elute The eluate was dissolved in 10L of 70% methanol at 40°C, and allowed to stand still. The crystal was filtered out. The crystallization was repeated twice and dried in the shade to obtain 2.95 g of needle crystal product (bergamot lactone content 98.4%).

Example Embodiment

[0026] Example 2:

[0027] Pulverize it to 80 meshes, take 10kg (bergamot lactone content 0.0045%), add 150L of 74% ethanol for reflux extraction for 4 hours, filter to obtain 155L of extract, add 60g of activated carbon, stir and decolorize at 45℃, pump the decolorizing solution into the pretreated Silica medium pressure column, elute with 8:1 petroleum ether / ethyl acetate mixture at a flow rate of 60ml / min, collect the eluate in 500ml portions, identify each component by TLC, and combine the bergamot lactone-containing segments for elution The eluate was dissolved in 12L of 73% methanol at 45°C, and allowed to stand still. The crystals were filtered out. The crystallization was repeated 3 times and dried in the shade to obtain 3.08 g of needle crystal products (the content of bergamot lactone 98.1%).

Example Embodiment

[0028] Example 3:

[0029] Crush the monocle to 100 mesh, take 10kg (bergamot lactone content 0.0048%), add 180L of 75% ethanol to reflux for 5 hours, filter to obtain 185L of extract, add 80g of activated carbon and stir at 50℃ for decolorization, pump the decolorizing solution into the pretreated Silica medium pressure column, eluted with 7:1 petroleum ether / ethyl acetate mixture at a flow rate of 60ml / min, collected eluates in 500ml portions, identified each component by TLC, and merged the bergamot lactone-containing segments for elution The eluate was dissolved in 15L of 75% methanol at 50°C, and allowed to stand. The crystals were filtered out. The crystallization was repeated 4 times and dried in the shade to obtain 3.14g of needle crystal products (bergamot lactone content 98.8%).

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Abstract

The invention relates to a method for separating and purifying bergapten. The processing steps include that radix angelicae pubescentis raw material is smashed into 60-100 meshes, 70-80% ethanol is used for reflux extraction, extract is added with active carbon with 0.5-1% of weight of raw material for stirring and destaining at the constant temperature of 40-50 DEG C, destaining solution is pumped into silica gel middle-pressure column subject to pre-treatment, 9-4:1 petroleum ether/ethyl acetate mixed liquor is used for eluting, eluent is collected in 500ml of each part, TLC detection is carried out, identical components are merged, bergapten eluent is obtained, 2-4 times volume of 70-80% methyl alcohol is used for flash melting at 40-50 DEG C, standing is carried out, crystal is filtered out, the process is repeated for 2-3 times, and drying in the shade is carried out, thus obtaining the product. By adopting the invention to produce bergapten, technology is simple, energy consumption is less, and purity is higher.

Description

Technical field: [0001] The invention relates to an extraction and purification process of bergamot lactone, in particular to a method for extracting and purifying bergamot lactone by using reflux extraction, silica gel chromatography and precipitation. Background technique: [0002] Bergamot Lactone (Bergapten) [0003] Alias: bergamot lactone, bergamot lactone, bergamot methyl ether, bergamotene [0004] Chemical name: 4-methoxyfuro[3,2-g]chromen-7-one [0005] Molecular formula: C 12 h 8 o 4 [0006] Molecular weight: 216.18952 [0007] [0008] Ingredient Classification: Furanocoumarins [0009] Physical properties: Bergamot lactone is white needle-like crystal with mercerization, melting point 188-190℃. Soluble in chloroform, slightly soluble in benzene, ethyl acetate and ethanol, insoluble in water. There is sublimation. Reflects blue fluorescence under UV light. [0010] Pharmacological effects: Bergamot lactone has optical activity on the skin, and its ...

Claims

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Application Information

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IPC IPC(8): C07D493/04
Inventor 刘东锋张翼杨成东
Owner NANJING ZELANG MEDICAL TECH
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