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Method for preparing germacrone

A technology for gemmanone and acetone, applied in the field of preparation of gemmanone, can solve the problems of inability to scale up the process, unstable instrument performance, small preparation amount, etc., and achieve the effects of improving production safety, good separation effect and large preparation amount

Inactive Publication Date: 2011-02-16
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chen Gang used high-speed countercurrent chromatography to separate and purify gemaconone and curcumadione in the volatile oil of Curcuma curcuma. The separation effect is good, but the cost is high, the performance of the instrument is unstable, the preparation volume is small, and the process cannot be scaled up.

Method used

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  • Method for preparing germacrone

Examples

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Effect test

Embodiment 1

[0023] Take Xing’an Rhododendron leaves, dry them in the shade, crush them into 40 meshes, weigh 8kg and put them into an ultrasonic extraction tank, add 40kg of acetone, and conduct ultrasonic extraction at 30°C for 3 times, each time for 2 hours, with a power of 300W and a frequency of 35kHz, and combine the acetone extracts , concentrated with a rotary evaporator to obtain acetone extraction extract; mix silica gel and alumina with a volume ratio of 5:1 and evenly pack it into a column, take acetone extraction extract and an equivalent amount of 180-mesh silica gel, mix evenly, pass through a 180-mesh sieve, and apply silica gel Chromatography on an alumina column, eluting with n-hexane-acetone at a gradient of 10:1, 5:1, 2:1, and 0:1, collecting the eluents separately, monitoring with HPLC, and combining the fractions containing gemmacone , concentrated with a rotary evaporator, dried at 40°C, mixed evenly with an equivalent amount of 300-mesh silica gel, ground through a 3...

Embodiment 2

[0025] Take Xing’an rhododendron leaves, dry them in the shade, crush them into 60 meshes, weigh 10kg and put them into an ultrasonic extraction tank, add 45kg of 95% ethanol, and conduct ultrasonic extraction at 35°C for 4 times, each time for 1.5 hours, with a power of 100W and a frequency of 40kHz, combined with ethanol extraction Concentrate the liquid with a rotary evaporator to obtain ethanol extraction extract; mix silica gel and alumina with a volume ratio of 7:1 and evenly pack it into a column, take ethanol extraction extract and an equivalent amount of 150-mesh silica gel, mix evenly, pass through a 150-mesh sieve, and Chromatography on a silica gel alumina column, eluting with n-hexane-ethyl acetate at a gradient of 10:1, 5:1, 2:1, and 0:1, collecting eluents separately, monitoring with HPLC, and combining Concentrate the genmacone part with a rotary evaporator, dry at 40°C, mix it with an equivalent amount of 300-mesh silica gel, grind it through a 300-mesh sieve, ...

Embodiment 3

[0027] Take warm curcuma, dry in the shade, crush 50 meshes, weigh 10kg and put it into an ultrasonic extraction tank, add 60kg of methanol, and conduct ultrasonic extraction at 35°C for 3 times, each time for 1 hour, with a power of 170W and a frequency of 40kHz. Combine the methanol extract, and use Concentrate with a rotary evaporator to obtain methanol extract; mix silica gel and alumina at a volume ratio of 8:1 and evenly pack in a column, take methanol extract and mix evenly with an equivalent amount of 200-mesh silica gel, pass through a 200-mesh sieve, and apply silica gel to alumina The column was chromatographed, and n-hexane-acetone was eluted with a gradient of 10:1, 5:1, 2:1, and 0:1, and the eluents were collected respectively, monitored by HPLC, and the fractions containing gemmacone were combined and used Concentrate with a rotary evaporator, dry at 40°C, mix evenly with an equivalent amount of 300-mesh silica gel, grind through a 300-mesh sieve, and sift throug...

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Abstract

The invention relates to a method for preparing germacrone, which belongs to the field of the preparation of traditional Chinese medicines. According to the method, the germacrone is extracted and prepared from raw materials which are rich in the germacrone. The preparation method comprises the following steps of: after primarily processing the raw materials which are rich in the germacrone, performing ultrasonic extraction by using an organic solvent at the temperature of below 45 DEG C; performing rotary evaporation and concentration to obtain extract; performing chromatography by using a silica gel-alumina composite column; performing gradient elution on the mixed solvent; recycling the solvent; and re-crystallizing by using petroleum ether-acetone or cyclohexane-ethanol to obtain the germacrone. By the preparation method, the germacrone has high yield; a closed system is adopted during extraction; solvent consumption is low; meanwhile, 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 gemaconone from raw materials rich in gemaconone. Background technique: [0002] Gemacone is a monocyclic sesquiterpene compound present in Geranium, Rhododendron and Zingiberaceae, used for asthma and cough relief. Gemacrone, the English name is Germacrone, molecular formula C 15 h 22 O, molecular weight 218.33, molecular structure formula is as follows: [0003] [0004] Xing'an Rhododendron, rightly called Manshanhong. Sexual taste is hard, warm. Return lung, spleen channel. It has the effect of relieving cough and eliminating phlegm, and is a commonly used medicine for treating acute and chronic bronchitis in Northeast China. The volatile oil contains a variety of sesquiterpenes, among which rhododendron is the main component with a large content. Its pharmacological and clinical studies have confirmed that rhododendron is t...

Claims

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Application Information

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IPC IPC(8): C07C49/647C07C45/78
Inventor 刘东锋郭琴杨成东
Owner NANJING ZELANG MEDICAL TECH
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