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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

AI Technical Summary

Problems solved by technology

In recent years, high-performance liquid chromatography has also been widely used to separate coumarin components, but the extraction effect on coumarins with few ester groups is not very good

Method used

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  • Method for extracting bergapten from radix angelicae pubescentis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Grind the lovage into 60 meshes, take 10kg (0.0046% of bergamot lactone content) and add 100L of 70% ethanol to reflux for extraction for 3 hours, filter to obtain 104L of extract, add 50g of activated carbon and stir at a constant temperature of 40°C for decolorization, and pump the decolorization solution into the pretreated Silica medium pressure column, use 9:1 petroleum ether / ethyl acetate mixture to keep the flow rate at 60ml / min for elution, collect the eluate in 500ml portions, identify the components by TLC, combine and elute with bergamot lactone The eluent was melted with 10L of 70% methanol at 40°C, left to stand, the crystals were filtered out, the crystallization was repeated twice, and dried in the shade to obtain 2.95 g of needle crystals (98.4% bergamot lactone content).

Embodiment 2

[0027] Grind the lovage into 80 mesh, take 10kg (0.0045% of bergamot lactone content) and add 150L of 74% ethanol to reflux for extraction for 4 hours, filter to obtain 155L of extract, add 60g of activated carbon and stir at a constant temperature of 45°C for decolorization, and pump the decolorization solution into the pretreated Silica gel medium pressure column, use 8:1 petroleum ether / ethyl acetate mixture to keep the flow rate at 60ml / min for elution, collect the eluate in 500ml portions, identify the components by TLC, and combine the bergamot lactone-containing segments for elution The eluent was melted with 12L of 73% methanol at 45°C, left to stand, the crystals were filtered out, the crystallization was repeated 3 times, and dried in the shade to obtain 3.08g of finished needle crystals (with a bergamot lactone content of 98.1%).

Embodiment 3

[0029] Grind the lovage into 100 meshes, take 10kg (0.0048% of bergamot lactone content) and add 180L of 75% ethanol to reflux for extraction for 5 hours, filter to obtain 185L of extract, add 80g of activated carbon and stir at a constant temperature of 50°C for decolorization, and pump the decolorization solution into the pretreated Silica gel medium-pressure column, use 7:1 petroleum ether / ethyl acetate mixture to keep the flow rate 60ml / min for elution, collect the eluate in 500ml each, identify each component by TLC, combine and elute with bergamot lactone The eluent was melted with 15L of 75% methanol at 50°C, left to stand, the crystals were filtered out, the crystallization was repeated 4 times, and dried in the shade to obtain 3.14g of finished needle crystals (98.8% bergamot lactone content).

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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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