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Method for preparing active monomer peonol from paniculate swallowwort root

A kind of active monomer, Xu Changqing's technology, applied in ether preparation, ether separation/purification, organic chemistry, etc., can solve the problems of no paeonol patent literature report, cumbersome preparation process, slow extraction speed, etc., and achieve low cost , wide application prospects and fast extraction speed

Inactive Publication Date: 2006-11-22
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has obvious disadvantages: slow extraction speed, high energy consumption, cumbersome preparation process, low yield, and sewage treatment problems due to the use of a large amount of water.
No patent literature report on the preparation of paeonol by ultrasonic extraction has been found through retrieval

Method used

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  • Method for preparing active monomer peonol from paniculate swallowwort root

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Bake 500g of the root of Xu Changqing at 60°C for 4 hours, crush it to 10 meshes, put the medicinal material powder into the reaction vessel of the ultrasonic extraction device, add 8 times the amount of petroleum ether with a boiling range of 30-60°C, and extract it ultrasonically for 2 hours (ultrasonic frequency 5000Hz). The filtered extract was refrigerated at 2°C for 4 hours to obtain pale yellow crystals, which were crude paeonol. Add 2 times the amount of 80% ethanol, control the temperature at 80°C, heat for 10 minutes, filter, and stand for crystallization for 5 hours to obtain nearly colorless crystals. The crystals were vacuum-dried at room temperature for 2 hours to obtain paeonol fine product, and the yield of paeonol was 1.24%.

Embodiment 2

[0019] Dry 500g of the root of Xu Changqing at 50°C for 4 hours, crush it to 30 meshes, put the medicinal material powder into the reaction vessel of the ultrasonic extraction device, add 9 times the amount of petroleum ether with a boiling range of 30-60°C, and extract it ultrasonically for 3 hours (ultrasonic frequency 5000Hz). The filtered extract was refrigerated at 3°C ​​for 6 hours to obtain pale yellow crystals, which were crude paeonol. Add 3 times the amount of 80% ethanol, control the temperature at 80°C, heat for 10 minutes, filter, and stand for crystallization for 4 hours to obtain nearly colorless crystals. The crystals were vacuum-dried at room temperature for 2 hours to obtain paeonol fine product, and the yield of paeonol was 1.31%.

Embodiment 3

[0021] Dry 500g of the root of Xu Changqing at 40°C for 4 hours, crush it to 50 meshes, put the medicinal material powder into the reaction vessel of the ultrasonic extraction device, add 10 times the amount of petroleum ether with a boiling range of 30-60°C, and extract it ultrasonically for 4 hours (ultrasonic frequency 5000Hz). The filtered extract was refrigerated at 2°C for 5 hours to obtain pale yellow crystals, which were crude paeonol. Add 4 times the amount of 80% ethanol, control the temperature at 80°C, heat for 10 minutes, filter, and stand for crystallization for 5 hours to obtain nearly colorless crystals. The crystal was vacuum-dried at room temperature for 2 hours to obtain paeonol fine product, and the yield of paeonol was 1.35%.

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Abstract

The invention relates to the preparation of paeonol, in particular to a method for preparing high-purity active monomer paeonol from Xu Changqing. The present invention adopts the dry root powder of the velvet vine plant Xu Changqing as a raw material, uses petroleum ether as an extraction solvent, uses ultrasonic extraction, and the ultrasonic frequency is 2000 Hz, 5000 Hz and 6000 Hz to extract for 1 hour or more, and the extract is refrigerated and crystallized to obtain paeonol The crude product is recrystallized with ethanol as a solvent, and after drying, the high-purity paeonol monomer can be obtained. The present invention uses Xu Changqing root as the raw material for paeonol preparation, and finds that the target component content in the extract is as high as 88.3%, and high-purity monomers can be obtained without column separation, and the preparation process is simple and easy to purify; using ultrasound as the extraction method has The advantages of fast extraction speed, high extraction rate and low equipment requirements are suitable for industrial production.

Description

technical field [0001] The invention relates to the preparation of paeonol, in particular to a method for extracting and preparing high-purity active monomer paeonol from the root of Xu Changqing by ultrasonic technology. Background technique [0002] Paeonol has obvious pharmacological activities such as antibacterial and anti-inflammatory, analgesic and sedative, lowering blood pressure, inhibiting atherosclerosis, promoting platelet aggregation and enhancing immune function. Paeonol-rich paeonol, Xu Changqing (the original plant is Cynanchum paniculatum (Bge.) Kitag.) and other traditional Chinese medicines are widely used clinically to treat thrombocytopenic purpura, bacillary dysentery and headache, etc. disease. [0003] Extraction of paeonol from plants usually adopts steam distillation: usually first use high-temperature steam to bring paeonol to the distillate, then extract paeonol in the distillate with ether, and then dry and distill off the ether, Finally, the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/253C07C41/34
Inventor 梁鑫淼张峰徐青肖红斌
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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