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Method for preparing high-purity lycaconitine

A kind of high-purity technology of Niuline, which is applied in the field of preparation of high-purity Niuline, can solve the problems of small preparation volume and cumbersome operation, and achieve the effects of large preparation volume, high separation efficiency and improved recovery rate

Inactive Publication Date: 2011-11-23
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0006] Chen Lishu et al. isolated Niubianjing from Kangding Aconitum root, extracted by percolation with hydrochloric acid solution, passed through a strong acid type styrene cation exchange resin column, extracted with ethanol reflux, acid dissolved, adjusted with alkali, extracted with chloroform, and eluted repeatedly with silica gel column. Niujianjing, the method is cumbersome to operate and the preparation amount is small, so it is only suitable for laboratory component analysis and identification

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  • Method for preparing high-purity lycaconitine

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Embodiment 1

[0014] Select the chloroform-methanol-0.2M HCl system to separate and purify Niujianjing in a countercurrent chromatograph, and first arrange the above-mentioned solvent components in a separatory funnel according to the volume ratio of 10:4:3, shake well, let stand, and wait for 30 minutes to balance , take the upper and lower phases respectively, the upper phase is used as the stationary phase, and the lower phase is used as the mobile phase, and 100 mg of phytamine crude extract powder is weighed and dissolved in 10 ml of the lower phase for use. Before sample injection, pump the stationary phase into the chromatographic column to fill the entire column, adjust the host speed to 900r / min, pump the mobile phase into the column at a flow rate of 3.0ml / min, and wait for the mobile phase to flow out from the liquid outlet And after the dynamic equilibrium of the two phases is established, the sample solution is injected into the chromatographic system through the injection valve...

Embodiment 2

[0016] Select the chloroform-methanol-0.5M HCl system to separate and purify Niujian alkaloid in a countercurrent chromatograph, and first arrange the above-mentioned solvent components in a separatory funnel according to the volume ratio of 16:5:7, shake it up, let it stand still, and wait for 30 minutes to balance , take the upper and lower phases respectively, the upper phase is used as the stationary phase, and the lower phase is used as the mobile phase, and 150 mg of Niuline crude extract powder is taken and dissolved in 10 ml of the lower phase for use. Before sample injection, pump the stationary phase into the chromatographic column to fill the entire column, adjust the host speed to 920r / min, pump the mobile phase into the column at a flow rate of 3.0ml / min, and wait for the mobile phase to flow out from the liquid outlet And after the dynamic equilibrium of the two phases is established, the sample solution is injected into the chromatographic system through the inje...

Embodiment 3

[0018] Select the chloroform-methanol-0.3M HCl system to separate and purify Niujianjing in a countercurrent chromatograph. First, the above solvent components are arranged in a separatory funnel according to the volume ratio of 8:2:5. , take the upper and lower phases respectively, the upper phase is used as the stationary phase, and the lower phase is used as the mobile phase, and 150 mg of phylloxine crude extract powder is weighed and dissolved in 15 ml of the lower phase for use. Before sample injection, pump the stationary phase into the chromatographic column to fill the entire column, adjust the host speed to 850r / min, pump the mobile phase into the column at a flow rate of 2.0ml / min, and wait for the mobile phase to flow out from the liquid outlet And after the dynamic equilibrium of the two phases is established, the sample solution is injected into the chromatographic system through the injection valve, and an ultraviolet detector is connected to the liquid outlet at...

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Abstract

The invention provides a method for preparing high-purity lycaconitine. The method provided by the invention comprises the following steps of: (1) preparing a solvent system with an upper phase which is a fixed phase and a lower phase which is a flowing phase; (2) filling a chromatograph column with the fixed phase and adjusting the rotating speed of a main machine to pump the flowing phase into the column; (3) dissolving 200-2000 mg of lycaconitine crude extract by using 20-100 ml of flowing phase; introducing the sample through a sample introducing valve and receiving a target component according to an ultraviolet map of a detector; and concentrating and crystallizing a flowing component to obtain a high-purity lycaconitine monomer. The lycaconitine prepared with the method provided by the invention can reach higher purity and the preparation method has the advantages of simplicity, high efficiency, low cost, easiness for reproduction and high separation and preparation capacity.

Description

Technical field: [0001] The invention relates to a method for separating and purifying the active ingredients of traditional Chinese medicines, in particular to a method for preparing high-purity Nitrine. Background technique: [0002] Diterpene alkaloids are a class of polycyclic nitrogen-containing compounds with relatively complex structures. They have strong toxicity and extensive biological activities. research hotspot. Most of the diterpene alkaloids are distributed in the genus Aconitum and Delphinium. In my country, there are about 170 species of Aconitum and nearly 120 species of Delphinium. They are widely distributed all over the country, especially in the southwest region. The most concentrated, many of which have already been commonly used Chinese herbal medicines in our country. Diterpene alkaloids are not only active and toxic constituents of such plants, but are also considered to be their characteristic chemical constituents. It has been reported in the li...

Claims

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Application Information

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IPC IPC(8): C07D221/22
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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