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Method for preparing high-purity laurotetanine with high speed reversed flow color spectrum method

A high-speed countercurrent chromatography and high-purity technology, which is applied in the field of high-purity hexapine prepared by high-speed countercurrent chromatography, achieves the effects of mild conditions, reduced chemical property changes, and short separation time

Inactive Publication Date: 2011-08-17
SHANGHAI INST OF PHARMA IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no complete set of theoretical basis for the selection of solvent system.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 5 kg of tempeh ginger was extracted with ethanol, the ethanol extract was extracted with n-butanol, and the n-butanol extracted part was roughly divided once with a silica gel column to obtain 15 grams of a mixture enriched with hexamethasone.

[0016] Accurately weigh 3.0 g of the mixture enriched with hexamethanine, dissolve the sample in the lower phase of the solvent system of chloroform:methanol:water (4:3:2), turn on the constant temperature circulator, set the temperature to 25°C, and use the solvent system The upper phase is the stationary phase, and the lower phase is the mobile phase. Use double pumps to pump the mobile phase and the stationary phase at the same time in equal proportions. When the solvent flows out from the outlet of the pipeline, stop pumping the stationary phase and set the flow rate of the mobile phase to 2ml / min. At the same time, start the host motor and adjust the speed to 800rpm. After more than ten minutes, the solvent in the column rea...

Embodiment 2

[0018] Accurately weigh 2.4 grams of the mixture enriched in hexamethasone in Example 1, dissolve the sample in the lower phase of the solvent system of chloroform:methanol:water (3.5:3:2), turn on the constant temperature circulator, set the temperature to 26°C, and The upper phase of the solvent system is the stationary phase, and the lower phase is the mobile phase. Use double pumps to pump the mobile phase and the stationary phase at the same time in equal proportions. When the solvent flows out from the outlet of the pipeline, stop pumping into the stationary phase and set the flow rate of the mobile phase. At the same time, start the motor of the main engine and adjust the speed to 750rpm. After ten minutes, the solvent in the column reaches a dynamic equilibrium, and only the mobile phase flows out from the outlet of the column. Inject the sample through the injector, set the wavelength to be 280nm, and the peak of hexaquabine appears in about 5 hours and 35 minutes afte...

Embodiment 3

[0020] Accurately weigh 2.6 grams of the mixture enriched in hexamethasone in Example 1, dissolve the sample in the lower phase of the chloroform:methanol:water (4:3:2.5) solvent system, turn on the constant temperature circulator, set the temperature to 27°C, and The upper phase of the solvent system is the stationary phase, and the lower phase is the mobile phase. Use double pumps to pump the mobile phase and the stationary phase at the same time in equal proportions. When the solvent flows out from the outlet of the pipeline, stop pumping into the stationary phase and set the flow rate of the mobile phase. At the same time, start the motor of the main engine and adjust the speed to 880rpm. After ten minutes, the solvent in the column reaches a dynamic equilibrium, and only the mobile phase flows out from the outlet of the column. Inject the sample through the injector, set the wavelength to be 280nm, and the peak of hexaquabine appears about 5 hours after the sample injectio...

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PUM

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Abstract

The invention discloses a method for preparing high-purity laurotetanine by high speed counter-current chromatography, comprising the steps of: preparing a solvent system for composing a stationary phase and a mobile phase; adjusting flow rate of the mobile phase; and adjusting the rotation speed of a motor. The method is characterized in that the solvent system is composed of chloroform, methanol and water with a volumetric ratio of (2-4):3:(2-2.5), the upper layer of solvent system is the stationary phase, and the lower layer of the solvent system is the mobile phase. The method has the advantages of mild separation conditions, high separation efficiency, short separation time, and high purity laurotetanine.

Description

technical field [0001] The invention relates to a method for preparing high-purity hexaline by high-speed countercurrent chromatography (HSCCC). Background technique [0002] Douchi ginger is the root and rhizome of Litsea cubeba (Lour.) Pers. It has the effects of expelling wind and cold, regulating qi and relieving pain. The alkaloid contained in it is a compound with strong pharmacological activity, which has a strychnine-like stimulating effect on the spinal cord. [0003] Hexapine exists in a very low amount in nature and contains a large amount of impurities, so a large number of researchers are exploring ideal separation and purification methods so far. The method that Masao et al. report in the literature Studies on the Alkaloids of Formosan Lauraceous Plants.V.Alkaloids of Litsea cubeba Persoon to extract hexaprine is as follows: 22.38 kg of tempeh ginger is extracted with ethanol, and the ethanol extract is extracted with 3% acetic acid, concentrated to a certain...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61K125/00A61K36/54C07D221/18
Inventor 朱超兰杨培明陈佳许海燕倪翔
Owner SHANGHAI INST OF PHARMA IND CO LTD
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