Method for preparing warburganal

A technology of wood aldehyde and wobo aldehyde, which is applied in the field of preparing wobo aldehyde, can solve the problem that wobo aldehyde has not been separated, and achieve the effects of improving production safety, less solvent consumption and good separation effect.

Inactive Publication Date: 2012-09-12
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

After searching, there is no report on the separation of Wuber wood aldehyde by silica gel alumina mixed column

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Take 1 kg of Wobo wood, grind it and extract it twice with methanol ultrasonically, and recover the reagent from the extract to obtain the extract, weigh silica gel (80 mesh) and neutral alumina (80 mesh) according to the volume ratio of 1:2, and mix them evenly Pack the column, mix the extract and an equal amount of silica gel evenly, and perform chromatography on a silica-alumina column, elute with a gradient of n-hexane-methanol (10:1, 8:1, 4:1, 1:1), and combine The fraction rich in Wuber wood aldehyde was recovered and the elution solvent was subjected to silica gel alumina (200 mesh) mixed column chromatography again, using n-hexane-methanol (50:1, 42:1, 30:1, 20: 1) Gradient elution, recovering the solvent, standing for crystallization, and then recrystallizing 4 times with petroleum ether-acetone at -4°C, filtering out the crystals, and freeze-drying to obtain 0.73g of the product.

Embodiment 2

[0016] Take 1kg of Wobur wood, crush it and extract it with acetone ultrasonically 4 times, recover the reagent from the extract to get the extract, weigh silica gel (120 mesh) and neutral alumina (120 mesh) according to the volume ratio of 8:1, and mix them evenly Pack the column, mix the extract and an equal amount of silica gel evenly, and perform chromatography on a silica-alumina column, elute with a gradient of n-hexane-methanol (10:1, 8:1, 4:1, 1:1), and combine The fraction rich in Wuber wood aldehyde was recovered and the elution solvent was subjected to silica gel aluminum oxide (300 mesh) mixed column chromatography again, and the mixture was chromatographed with n-hexane-methanol (50:1, 42:1, 30:1, 20: 1) Gradient elution, recovering the solvent, standing for crystallization, and then recrystallizing with cyclohexane-ethanol at -10°C, filtering out the crystals, and freeze-drying to obtain 0.68g of the product.

Embodiment 3

[0018] Take 10kg of Wobo wood, after crushing, ultrasonically extract 3 times with a mixed solvent of methanol and ethanol, and recover the reagent from the extract to obtain an extract. Weigh silica gel (100 mesh) and neutral alumina (100 mesh) according to a volume ratio of 3:1. mesh), mix evenly and pack into a column, mix the extract and an equal amount of silica gel evenly, and perform chromatography on a silica gel-alumina column, using n-hexane-methanol (10:1, 8:1, 4:1, 1:1) Gradient elution, combined the fractions rich in Wobbe wood aldehyde, recovered the elution solvent, and applied to silica gel alumina (300 mesh) mixed column chromatography again, using n-hexane-methanol with (50:1, 42:1, 30 :1, 20:1) gradient elution, recover the solvent, stand to crystallize, and then recrystallize twice with cyclohexane-ethanol at -8°C, filter out the crystals, and freeze-dry to obtain 6.4g of the product.

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Abstract

The invention relates to a method for preparing warburganal and belongs to the field of preparation of traditional Chinese medicines. According to the method, warburganal is extracted from raw materials rich in warburganal. The method comprises the following steps of grinding the raw materials rich in warburganal, performing ultrasonic extraction by adding a hydrophilic organic solvent, recycling the organic solvent to obtain an extract, performing chromatographic separation by using a silica gel alumina mixed column for two times, performing gradient elution by adding the mixed solvent, recycling the solvent, standing a solution for crystallization, and performing re-crystallization by adding petroleum ether-acetone or cyclohexane-methanol to obtain the product. The method has the advantages that the yield is high, a closed system is adopted in the extracting process, the consumption of the solvent is reduced, and the production safety is improved.

Description

technical field [0001] The invention belongs to the field of traditional Chinese medicine pharmacy, and relates to a method for preparing weber wood aldehyde from raw materials rich in weber wood aldehyde. Background technique [0002] Weber wood aldehyde is a kind of sesquiterpene aldehyde compound existing in the plants of Cinnamonaceae, Polygonaceae and Aniseaceae. Warburg wood aldehyde, the English name is Warburganal, the molecular formula is C15H22O3, the molecular weight is 250.34, and the molecular structure is as follows: [0003] . [0004] Wobur wood aldehyde has multiple pharmacological effects. It has antifeedant effect on African armyworm and potato aphid. In addition, it also has strong anti-fungal activity. It can inhibit the growth of Saccharomyces cerevisiae and alcohol fermentation. Reversed by acid, the MIC for Saccharomyces cerevisiae, Candida cystogenes, and Sclerotinia soybean was 3.13 μg / mL; the MIC for Schizosaccharomyces pombe and Hansenula abno...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/46C07C45/78
Inventor 刘东锋吴艳波
Owner NANJING ZELANG MEDICAL TECH
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