Preparation method of corynoloxine

The technology of Cordyloxacin base and Viola vulgaris is applied in the biological field, can solve the problems of pollution, low extraction efficiency, low product yield and the like, and achieves the effects of simple operation, high extraction efficiency and high product purity.

Inactive Publication Date: 2013-12-11
NANJING TONGZE AGRI SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 corydalis loxine

Method used

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  • Preparation method of corynoloxine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take 3kg of dried chrysalis, 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 simultaneously feed chloroform as entrainer, the flow rate is 1ml / min / g, Raw materials were extracted at a temperature of 45°C, a pressure of 22Mpa, and an extraction time of 2 hours. The analyzed extract was dissolved in 70% acetone solution, and the calcium peroxide short column was used to collect and concentrate the liquid through the column to obtain an extract. Take chloroform, methanol, water, mix according to 3:2:2, take the upper phase as the stationary phase, the host speed is 800rpm, the lower phase is the mobile phase, the flow rate is 2ml / min, the ultraviolet detector is online monitoring, and the collected fraction is dried under reduced pressure , to obtain 1.1 g of Corydalis loxine, detected by HPLC, with a content of 98.2%.

Embodiment 2

[0017] Take 3kg of dried chrysanthemum japonicus, crush it into 40 meshes, put it in a CO2 supercritical extraction tank, feed liquid CO2, the flow rate is 2ml / min / g raw material, and feed chloroform at the same time as entrainer, the flow rate is 2ml / min / g, Raw materials were extracted at a temperature of 50°C, a pressure of 25Mpa, and an extraction time of 3 hours. The analyzed extract was dissolved in 70% acetone solution, and the calcium peroxide was short-columned. The collected liquid was concentrated to obtain an extract. Take chloroform, methanol, water, mix according to 5:3:4, 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 obtain 1.2 g of corydalis loxine, which was detected by HPLC with a content of 97.3%.

Embodiment 3

[0019] Take 3kg of dried chrysalis, crush it into 20 meshes, put it in a CO2 supercritical extraction tank, feed liquid CO2, the flow rate is 4ml / min / g raw material, and simultaneously feed chloroform as entrainer, the flow rate is 2ml / min / g, Raw materials were extracted at a temperature of 30°C, a pressure of 15Mpa, and an extraction time of 1 hour. The analyzed extract was dissolved in 70% acetone solution, and the calcium peroxide short column was used to collect and concentrate the liquid through the column to obtain an extract. Take chloroform, methanol, water, mix according to 7:5:5, take the upper phase as the stationary phase, the host speed is 900rpm, the lower phase is the mobile phase, the flow rate is 1ml / min, the ultraviolet detector is online monitoring, and the collected fraction is dried under reduced pressure , to obtain 1.3g of Corydalis loxine, which was detected by HPLC with a content of 97.2%.

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Abstract

The invention discloses a preparation method of corynoloxine, which is simple and easy to operate and less in pollution. The preparation method of the corynoloxine comprises the following steps: (1) preparing dry incised corydalis herb, smashing into 20-80 meshes, extracting in a CO2 supercritical extraction tank, introducing liquid CO2 at a flow rate of 1-4ml / min for one gram raw material while introducing chloroform as a cosolvent at a flow rate of 1-4ml / min / g, and resolving to obtain an extractant, wherein a raw material extraction temperature is 30-50 DEG C, pressure is 15-25MPa, and extraction time is 1-3 hours; and 2) dissolving the extractant with a 70% acetone solution, passing through a calcium peroxide short column, collecting liquid passing through the short column and concentrating, then separating by adopting a high-speed countercurrent chromatographic instrument, carrying out online monitoring by adopting an ultraviolet detector, collecting fractions, and carrying out reduced pressure drying, thus the corynoloxine is obtained. When the preparation method of the corynoloxine is adopted for preparing the corynoloxine, the obtained corynoloxine product is high in purity, and industrial production is easy to realize.

Description

technical field [0001] The invention belongs to the field of biotechnology, and in particular relates to a preparation method of corydalis loxine. Background technique [0002] Corydalis loxine, CAS registration number 31470-65-2, molecular formula C21H19NO5, molecular weight 365.39, molecular structural formula: [0003] [0004] Zihuayu Dengcao is the whole plant and root of Corydalis papaeae, the whole plant contains a variety of alkaloids: protoopine, sanguinarine, coptisine, corydine, corydine losingine, Corydoline, Corydoline, Acetylcoryloline, Acetylisocordyline, Coryline, Violetine, Methyl Violet, Corydoline, N-Formyl Leaf corydine, hua corydine, sterner's corydine, heterobicuculline boracine, qingfengmenine, remote mountain cordyline and vine bicuculline l-corydine, etc. For the treatment of scabies, vicious insect sores, poisonous poison, knife wounds, arthralgia in the ankles and other diseases. [0005] According to the literature search, the preparation me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/22
CPCY02P20/54
Inventor 杨存
Owner NANJING TONGZE AGRI SCI & TECH
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