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Method for separation purification of Chinese magnoliavine fruit monomers by using dynamic axial compression column

A technology of axial compression and schisandra, applied in the field of biochemistry, can solve the problems of high performance requirements of gradient elution equipment, large influence of solvent residues, high toxicity, etc., to achieve easy control of product quality, low equipment performance requirements, and short production cycle. Effect

Active Publication Date: 2013-09-04
江苏迪沃特仪器设备科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a method for separating and purifying Schisandra chinensis monomer with a dynamic axial compression column, which can solve the problem of prior art through chromatographic column chromatography, and then use acetonitrile and water gradient elution to pass through reversed-phase chromatographic column , it needs to pass through the chromatographic column twice to generate a large amount of solvent, which consumes a lot of energy and takes a long time; moreover, acetonitrile is highly toxic and has a great influence on the residual solvent; gradient elution requires high equipment performance.

Method used

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  • Method for separation purification of Chinese magnoliavine fruit monomers by using dynamic axial compression column
  • Method for separation purification of Chinese magnoliavine fruit monomers by using dynamic axial compression column
  • Method for separation purification of Chinese magnoliavine fruit monomers by using dynamic axial compression column

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Embodiment 1

[0031] The method for separating and purifying Schisandra chinensis monomer with a dynamic axial compression column comprises the following steps:

[0032] (1) Preparation of mobile phase: Prepare the mobile phase with n-hexane, ethyl acetate and isopropanol in a volume ratio of 95:2:3 as the sample eluent;

[0033] (2) Dissolution and filtration: Dissolve 10 g of Schisandra chinensis crude product in a mixed solution of n-hexane, ethyl acetate and isopropanol with a volume ratio of 3:1:6, filter it with a 0.45 μm organic filter membrane after ultrasonication, and filter the filtrate with step (1 ) to dilute the prepared mobile phase into a sample with a concentration of 0.5g / ml; among them, the crude product of Schisandra chinensis is boiled and filtered by the medicinal material of Schisandra chinensis, and the obtained dregs are purified and filtered with 80% ethanol to obtain the filtrate. After all the ethanol is volatilized, the remaining substance is precipitated with w...

Embodiment 2

[0040] The method for separating and purifying Schisandra chinensis monomer with a dynamic axial compression column comprises the following steps:

[0041] (1) Mobile phase preparation: prepare mobile phase with n-hexane, ethyl acetate, and isopropanol in a volume ratio of 70:23:7 as the sample eluent;

[0042] (2) Dissolution and filtration: Dissolve 100g of Schisandra chinensis crude product in a mixed solution of ethyl acetate and isopropanol with a volume ratio of 1:1, filter it with a 0.45μm organic filter membrane after ultrasonication, and use the mobile phase prepared in step (1) for the filtrate Diluted to a sample concentration of 0.4g / ml;

[0043] (3) Packing of dynamic axial compression column: Homogenize 2000g of 200~800 mesh polar silica gel filler with the mobile phase prepared in step (1) to obtain a homogenate, and send the homogenate into a dynamic axial compression column with a diameter of 150mm , after the mobile phase is discharged, the chromatographic f...

Embodiment 3

[0049] The method for separating and purifying Schisandra chinensis monomer with a dynamic axial compression column comprises the following steps:

[0050] (1) Preparation of mobile phase: Prepare the mobile phase with n-hexane, ethyl acetate, and isopropanol in a volume ratio of 60:30:10 as the sample eluent;

[0051] (2) Dissolution and filtration: Dissolve 500g of Schisandra chinensis crude product with n-hexane solution, filter it with a 0.45μm organic filter membrane after ultrasonication, and dilute the filtrate with the mobile phase prepared in step (1) to a sample with a concentration of 0.28g / ml;

[0052] (3) Packing of dynamic axial compression column: Homogenize 8000g of 200~800 mesh polar silica gel filler with the mobile phase prepared in step (1) to obtain a homogenate, and send the homogenate into a dynamic axial compression column with a diameter of 300mm , after the mobile phase is discharged, the chromatographic filler is compacted to complete the filling of ...

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Abstract

The present invention discloses a method for separation purification of Chinese magnoliavine fruit monomers by using a dynamic axial compression column. The method comprises the following steps: mobile phase preparation, dissolution filtration, dynamic axial compression column filling, system balancing, elution separation and concentration. According to the present invention, a plurality of monomers can be obtained during a separation purification process, purities detected by a liquid chromatography method are more than 98.5%, and yields are more than 98%; the process is simple, and the used organic solvents have characteristics of low price, low consumption and capability of recycling; an ultraviolet detector is adopted to perform online monitoring, operation is simple, efficiency is high, and product quality is easy to control; and isocratic elution is performed, performance requirements on equipment are low, a production cycle is short, and efficient Chinese magnoliavine fruit monomer separation purification from the laboratory to the industry can be easily achieved.

Description

technical field [0001] The invention relates to the field of biochemistry, in particular to a method for separating and purifying Schisandra chinensis monomer by using a dynamic axial compression column. Background technique [0002] Schisandra, commonly known as Shanhuajiao, Scale Duozi, Medicinal Schisandra, Mianteng, Wumeizi, etc., ancient medical books call it Chuzhu, Xuanji, Huiji, which was first listed in the top grade of Shennong’s Herbal Classic. The functions of Schisandra are: 1. The extract of Schisandra chinensis and alcohol A can reduce the spontaneous activity of mice, and have analgesic effect and muscle relaxation effect; 2. Schisandra alcohol extract and Schizandrin A, B, C, Alcohol A, Alcohol B, Ester A, Ester B, etc. have obvious protective effects on animal liver cell damage caused by chemical poisons; 3. Schisandrin, Schizandrin C, deoxyschisandrin, etc. all have inhibitory effect on isolated dog mesenteric artery contraction, and can increase the isol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/10C07C43/21C07C43/23C07C41/36C07D317/70C07D493/04
Inventor 孟强孙娟戴士俊张俊张云海范金豹沈红艳周亮亮
Owner 江苏迪沃特仪器设备科技有限公司
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