Process for extracting curcumenol by molecular distillation method

A technology of molecular distillation and curcumol, which is applied in the direction of organic chemistry, can solve the problems of unsatisfactory yield and purity, and achieve high-purity results

Inactive Publication Date: 2015-11-18
海门德思行药业科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But it is not very ideal in terms of yield and purity

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  • Process for extracting curcumenol by molecular distillation method

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Embodiment 1

[0020] A kind of technique of extracting curcumol by molecular distillation of the present invention, molecular still 1 is cleaned with ethanol in advance, dry, add 500 grams of commercially available curcuma oil in feed unit 3, first under the vacuum degree of 1.3mbar at normal temperature Degas for 25 minutes, until the zedoary oil in the feed unit 3 no longer bubbles, turn on the condensed water and the oil bath heater, the condensation temperature is -5°C, the oil bath heating temperature is 70°C, and after the temperature is stable, turn on the scraping and stirring , adjust the rotating speed to be 150rpm, and the vacuum is 1.2mbar. Then, slowly add turmeric oil to the distiller dropwise from the feed unit 3, and control the flow rate to be 1.7 drops / second. After the dropwise addition, collect 290 grams of directly condensed fractions, 110 grams of externally condensed distillate, 40 grams of unevaporated residue, and 7 grams of degassed light components;

[0021] After...

Embodiment 2

[0023] A kind of technique of extracting curcumol by molecular distillation of the present invention, molecular still 1 is cleaned with ethanol in advance, dry, add 500 grams of commercially available curcuma oil in feed unit 3, first under the vacuum degree of 1.5mbar at normal temperature Degas for 28 minutes until the zedoary oil in the feeding unit 3 no longer bubbles, turn on the condensed water and the oil bath heater, the condensation temperature is 0°C, and the oil bath heating temperature is 75°C. After the temperature is stable, turn on the scraping and stirring. Regulating rotating speed is 180rpm, and vacuum is 1.2mbar, then, slowly add zedoary oil to distiller dropwise from feed unit 3, control flow rate is 2 drops / second, after dropwise, collect direct condensation distillate 280 grams, outside Set 110 grams of condensed fraction, 45 grams of unevaporated residue, and 8 grams of degassed light components;

[0024] After 45 grams of the unevaporated residual porti...

Embodiment 3

[0026] A kind of technique of extracting curcumol by molecular distillation of the present invention, molecular still 1 is cleaned with ethanol in advance, dry, add 500 grams of commercially available curcuma oil in feed unit 3, first under the vacuum degree of 1.8mbar at normal temperature Degas for 30 minutes, until the zedoary oil in the feeding unit 3 no longer bubbles, turn on the condensed water and the oil bath heater, the condensation temperature is 5°C, and the oil bath heating temperature is 80°C. After the temperature is stable, turn on the scraping and stirring. Regulating rotating speed is 200rpm, and vacuum degree is 1.3mbar, then, slowly add zedoary oil to distiller dropwise from feed unit 3, control flow rate is 2.3 drop / second, after dropwise, collect direct condensed distillate 298 grams, outside Set 117 grams of condensed fraction, 48 grams of unevaporated residue, and 9 grams of degassed light components;

[0027] After 48 grams of the unevaporated residual...

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Abstract

The invention discloses a process for extracting curcumenol by a molecular distillation method. The process comprises the following steps of: adding zedoary oil into a feeding unit; firstly carrying out normal-temperature degassing under vacuum degree, and then opening condensed water and an oil-bath heater; after the temperature is stable, starting scraping-film stirring; then dripping the zedoary oil into a distiller; after the dripping is finished, collecting direct condensation fractions, external condensation fractions, unevaporated residual parts and degassed light components and losing; after the unevaporated residual parts are placed for one day, precipitating a great amount of crystals, using petroleum ether to carry out milliliter pulping, filtering, and drying to obtain white crystal; using alcohol with the mass concentration being 95% to recrystallize the crystal, and obtaining the curcumenol crystal with the gas chromatography GC being larger than 99%. The process disclosed by the invention has the advantages that according to the molecular distillation principle, the zedoary oil is treated by molecular distillation, the liquid part is condensed into liquid on an internal condenser by short-process distillation, then the discharged material is discharged, the zedoary oil can be rapidly separated from the curcumenol, and by combination with the recrystallizing technology, the curcumenol with high purity can be obtained.

Description

technical field [0001] The invention relates to a process for extracting curcumol by molecular distillation. Background technique [0002] Curcumol is one of the important components of the volatile oil of traditional Chinese medicine Zezhu (Pengzezhu, Guangxi Curcuma, Wenyujin). Since the 1970s, it has been used in the treatment of cervical cancer and has achieved certain curative effect. In recent years, pharmaceutical workers have conducted extensive research on curcumol. In terms of pharmacological effects, curcumol has significant antitumor effects, as well as antibacterial and antiviral effects. [0003] However, due to the difficulty in large-scale extraction and separation of curcumol, the pharmacodynamic research and clinical application of curcumol cannot be deepened. The traditional method is to extract Zezhu with methanol or water, then carry out steam distillation, and then recrystallize with ethyl acetate or absolute ethanol. However, the yield and purity a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/08
CPCC07D493/08
Inventor 朱伟
Owner 海门德思行药业科技有限公司
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