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Preparation method of corynoxine

A drying and flow technology, applied in the biological field, can solve the problems of poor process reproducibility, low product yield, low extraction efficiency, etc., and achieve the effects of high extraction efficiency, high product purity, and simple method operation.

Inactive Publication Date: 2013-12-18
NANJING BIAOKE BIO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This type of method has low extraction efficiency, low product yield, poor process reproducibility, serious pollution, and is not suitable for the preparation of high-purity coronocine base

Method used

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  • Preparation method of corynoxine

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Experimental program
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Effect test

Embodiment 1

[0017] Take 2kg of dried Uncaria macrophyllum, crush it into 60 meshes, put it in a CO2 supercritical extraction tank, feed liquid CO2, the flow rate is 3ml / min / g raw material, and feed chloroform as entrainer at the same time, the flow rate is 2ml / min / g , the raw material extraction temperature is 45°C, the pressure is 20Mpa, the extraction time is 2h, the analytical extract is dissolved in 75% methanol solution, and the liquid is collected by a short column of neutral alumina (basic alumina particle size 120 mesh) and concentrated to obtain an extract. Take chloroform, methanol, water, mix according to 3:2:3, take the upper phase as the stationary phase, the host speed is 850rpm, the lower phase is the mobile phase, the flow rate is 3ml / min, the ultraviolet detector is online monitoring, and the collected fraction is dried under reduced pressure , to get 2.9g coronocine base, detected by HPLC, the content was 98.5%.

Embodiment 2

[0019] Take 2kg of dried Uncaria macrophyllum, crush it into 20 meshes, put it in a CO2 supercritical extraction tank, feed liquid CO2, the flow rate is 2ml / min / g raw material, and feed chloroform as entrainer at the same time, the flow rate is 2ml / min / g , the raw material extraction temperature is 30°C, the pressure is 25Mpa, and the extraction time is 3h. The analytical extract is dissolved in 80% methanol solution, passed through a short column of neutral alumina (basic alumina particle size 120 mesh) to collect and concentrate the liquid in the lower column to obtain an extract. Take chloroform, methanol, water, mix according to 5:5:7, take the upper phase as the stationary phase, the speed of the host is 800rpm, the lower phase is the mobile phase, the flow rate is 3ml / min, the ultraviolet detector is online monitoring, and the collected fraction is dried under reduced pressure , to get 3.1g coronocine base, detected by HPLC, the content was 97.1%.

Embodiment 3

[0021] Take 2kg of dried Uncaria macrophyllum, crush it into 80 meshes, put it in a CO2 supercritical extraction tank, feed liquid CO2, the flow rate is 5ml / min / g raw material, and feed chloroform as entrainer at the same time, the flow rate is 1ml / min / g , the raw material extraction temperature is 50°C, the pressure is 23Mpa, the extraction time is 2h, the analytical extract is dissolved in 90% methanol solution, and the liquid is collected by a short column of neutral alumina (basic alumina particle size 120 mesh) and concentrated to obtain an extract. Take chloroform, methanol, and water, mix according to 4:3:5, take the upper phase as the stationary phase, and the lower phase as the mobile phase, the host speed is 900rpm, the flow rate is 2ml / min, the ultraviolet detector is monitored online, and the collected fraction is dried under reduced pressure , to get 3.3g coronocine base, detected by HPLC, the content was 97.1%.

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Abstract

The invention discloses a preparation method of corynoxine, which is simple to operate and small in pollution. The method comprises the following steps: 1) taking dry Uncaria macrophylla, pulverizing into 20-80 meshes, extracting in a CO2 supercritical extraction tank at 30-50 DEG C under the pressure of 15-30 MPa for 1-3 hours, introducing liquid CO2 at the rate of 1-5 ml / minute / g raw material while introducing chloroform as an entrainer at the rate of 1-5 ml / minute / g, and resolving to obtain the extract; and 2) dissolving the extract in a methanol solution, passing through an aluminum peroxide short column, collecting the liquid, concentrating, separating with a high-speed counter-current chromatograph, carrying out on-line monitoring with an ultraviolet detector, collecting the fraction, and drying under reduced pressure. The method is suitable for preparing high-purity corynoxine.

Description

technical field [0001] The invention belongs to the field of biotechnology, and in particular relates to a preparation method of kronoxine. Background technique [0002] Kornosine is an indole alkaloid, CAS registration number 6877-32-3, molecular formula C22H28N2O4, molecular weight 384.46, molecular structural formula: [0003] [0004] Uncaria uncariae is a plant of Rubiaceae, bitter in taste, astringent in taste, cool in nature, clearing fire and detoxification, reducing swelling and pain, dispelling wind, ventilating blood, and lowering blood pressure [0005] According to the literature search, the preparation method of kronosine mostly adopts organic reagent extraction and silica gel column separation. This type of method has low extraction efficiency, low product yield, poor process reproducibility, serious pollution, and is not suitable for the preparation of high-purity coronocine base. Contents of the invention [0006] The technical problem to be solved by...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/20
CPCY02P20/54
Inventor 张金芳万冬梅
Owner NANJING BIAOKE BIO TECH
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