Phellodendrine monomer and preparation method of salt thereof

A technology for Phellodendron alkaloids and monomers is applied in the field of preparation of Phellodendron alkaloids monomers and salts thereof, which can solve the problems of complicated operation, low product yield and high production cost, and achieves low technical level requirements, simple technological process and high production cost. reduced effect

Inactive Publication Date: 2013-09-18
SOUTHWEST JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] For the obtaining of cortex base monomer and its salt, at present, traditional methods such as solvent method and repeated silica gel column chromatography are mainly used to separate. Unable to meet the needs of further development and utilization
In recent years, there has been a method for preparing phellodine salt monomer by liquid chromatography separation method, as No. 200910311304.9 Chinese patent application discloses a method for adopting preparative high performance liquid chromatography to separate phellodine salt monomer, which can obtain high High-quality cortex base salt monomer, but the preparative high-performance liquid chromatograph and its accessories used in this process are quite expensive, resulting in very high production costs; and the process has a long preparation cycle and cumbersome operation, which is not conducive to the promotion of industrialization

Method used

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  • Phellodendrine monomer and preparation method of salt thereof
  • Phellodendrine monomer and preparation method of salt thereof
  • Phellodendrine monomer and preparation method of salt thereof

Examples

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Comparison scheme
Effect test

Embodiment 1

[0039] A preparation method for Phellodendron monomer, comprising the following steps:

[0040] (1) Extraction of Phellodendronine

[0041] Get dry Cortex Phellodendri medicinal material 2kg, prepare its KCl solution that the mass fraction of 8 times volume is 3.0%, and the pH value of chlorine salt solution is adjusted to 2, when adjusting the pH value of KCl solution, the acid that adopts is hydrochloric acid, extracts 2 times, 48 ​​hours each time, combine the extracts and discard the drug residues;

[0042] (2) Enrichment of Phellodendronine

[0043] The combined extract is adsorbed by non-polar polystyrene type macroporous adsorption resin column chromatography, the model of this macroporous adsorption resin is D101 type macroporous resin, and the volume of macroporous adsorption resin is 1Kg with the dry Cortex Phellodendri medical material weight ratio: 1L, the adsorption rate is controlled at 2.0BV / h; after the adsorption is completed, first use 1.0BV of water to elu...

Embodiment 2

[0049] A preparation method for Phellodendron monomer, comprising the following steps:

[0050] (1) Extraction of Phellodendronine

[0051] Get dry Cortex Phellodendri medicinal material 2kg, prepare its 10 times of volume mass fraction as the NaCl solution of 4.0%, and the pH value of the chloride salt solution is adjusted to 2.5, when regulating the pH value of the chloride salt solution, the acid adopted is sulfuric acid, Extract twice, 48 hours each time, combine the extracts, and discard the drug residues;

[0052] (2) Enrichment of Phellodendronine

[0053] The combined extract is adsorbed by non-polar polystyrene type macroporous adsorption resin column chromatography, the model of this macroporous adsorption resin is AB-8 type macroporous resin, the volume of macroporous adsorption resin and the weight ratio of the dried Cortex Phellodendri medicinal material is 1Kg: 1.25L, the adsorption rate is controlled at 2.5BV / h; after the adsorption is completed, first wash wi...

Embodiment 3

[0059] A preparation method for Phellodendron monomer, comprising the following steps:

[0060] (1) Extraction of Phellodendronine

[0061] Get dry Cortex Phellodendri medicinal material 5kg, the mass fraction of its 9 times volume of preparation is 5.0% CaCl 2 solution, and the CaCl 2 The pH of the solution was adjusted to 3, and the CaCl 2 When the pH value of the solution is used, the acid used is nitric acid, and the extraction is performed twice, each time for 48 hours, the extracts are combined, and the medicinal residues are discarded;

[0062] (2) Enrichment of Phellodendronine

[0063] The merging extract is adsorbed by nonpolar polystyrene type macroporous adsorption resin column chromatography, the model of this macroporous adsorption resin is HP20 type macroporous resin, and the macroporous adsorption resin volume is 1Kg with the dry Cortex Phellodendri medical material weight ratio: 1.5L, the adsorption rate is controlled at 3.0BV / h; after the adsorption is co...

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Abstract

The invention belongs to the technical field of natural medicine extraction, and relates to a phellodendrine monomer and a preparation method of salt thereof. The method comprises the steps of: preparing the phellodendrine monomer through acid chloride solution extraction, macroporous adsorption resin enrichment, alumina column chromatographic purification and the like; and recrystallizing the phellodendrine monomer so as to obtain a phellodendrine salt monomer. The method has the advantages of low preparation cost, short period and high prepared product purity, and is convenient to operate.

Description

technical field [0001] The invention relates to a method for preparing a phellodine monomer and a salt thereof, and belongs to the technical field of natural medicine extraction. Background technique [0002] Phellodendron Phellodendri is the dry bark of Phellodendron chrysalis or Cortex Phellodendron, which is a commonly used traditional Chinese medicine. Cortex Phellodendron contains a higher amount of alkaloids, including benzylisoquinoline alkaloids such as berberine (Berberine), palmatine (Palmatine), etc. Alkali (magnoflorine), etc. The main pharmacological activity of benzyl isoquinoline alkaloids such as berberine and palmatine is antibacterial activity, while aporphyrin alkaloids such as cortex phellodendriline and magnoline have activities such as lowering blood pressure and nerve blocking. Cortex Phellodendron is the characteristic component and important active ingredient of Cortex Phellodendri. Modern pharmacological studies have shown that Cortex Phellodendro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D455/03
Inventor 周先礼罗鸿肖峰黄帅单连海王萃娟
Owner SOUTHWEST JIAOTONG UNIV
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