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Purification method and crystal form of berberine or berberine salt

A purification method and technology of berberine, applied in the field of purification of berberine or its salt, can solve the problems of inability to meet standards, low success rate, low efficiency and the like

Active Publication Date: 2020-05-29
JIANGXI FUSHINE PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solvent recrystallization method defect of berberine hydrochloride at present: 1) efficiency is low, need multiple recrystallization
2) Poor repeatability, which is extremely related to the source and purity of raw materials
3) The success rate is low, and for crude products containing various impurities, they often fail to meet the standards
In order to improve the safety of drugs and reduce the cost of drugs, it is ideal to be able to directly prepare products with a single impurity content of less than 0.1%. or preparation method

Method used

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  • Purification method and crystal form of berberine or berberine salt
  • Purification method and crystal form of berberine or berberine salt
  • Purification method and crystal form of berberine or berberine salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] 38.3 g of berberine sulfate (0.10 mmol, 87% purity) was dissolved in 2.0 liters of water to obtain a brown solution, and 0.10 liter of 1N aqueous sodium hydroxide solution was added at room temperature. With stirring at room temperature, 0.01 liter (a small amount) of acetone was added dropwise. After the pale yellow crystals were precipitated, the stirring was continued for 2 hours, and the light yellow berberine acetone adduct was obtained by filtration. The single crystal structure of the obtained acetone adduct is as follows figure 1 Shown (single crystal analysis using Bruker Apex diffractometer, purchased from Bruker AXS Inc TM (Madison, Wisconsin). Diffraction data were collected at 23°C using a Mo source). The XRD diffraction spectrum pattern of the acetone adduct obtained is shown in figure 2 (performed using a Bruker D8 diffractometer purchased from Bruker AXS Inc TM (Madison, Wisconsin), the detection conditions are: the sample (about 10 mg) is mounted ...

Embodiment 2

[0090] 32g of berberine hydrochloride (purity: 90%) and 1280ml of methanol, about 20 ℃ began to drop 428ml of 0.2N NaOH, to obtain a brown clear liquid. After dropping, stir for 10 minutes and filter, and add 172ml of acetone dropwise to the filtrate. After dropping, lower the temperature to 10-15°C and stir for 2 hours, filter, and dry at room temperature to obtain the berberine acetone complex, the XRD data and figure 2 Basically the same. Put the whole batch of wet product and 1600ml of water into the 2000ml bottle, and add 160ml of 1mol / L hydrochloric acid dropwise. After dropping, raise the temperature to 80-100°C to obtain a yellow liquid and keep it warm for 10 minutes. After the heat preservation is completed, the temperature is lowered to below 30°C to obtain a yellow needle-like or yellow fibrous solid, which is filtered by suction, rinsed with water, drained, that is, 27.2g of berberine hydrochloride, and dried to obtain 27.2g of the product, with a yield of 85% ...

Embodiment 3

[0092] Utilize berberine acetate that purity is 86% to replace " 38.3 grams berberine sulfate " in embodiment 1, molar weight is identical, carry out same reaction, the berberine hydrochloride yield that obtains at last is 85% purity 99.85 %, the simple impurity content is lower than 0.1%.

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Abstract

The invention discloses a purification method of berberine or berberine salt, wherein the method comprises the steps: converting a raw material mainly containing berberine or berberine salt I into anacetone adduct of berberine, and converting the acetone adduct of berberine into berberine salt II to obtain the product berberine salt II or berberine. The invention also discloses an acetone adductcrystal form of berberine. The purification method is adopted; by converting the raw material containing berberine or berberine salt into the berberine acetone adduct and then converting the berberineacetone adduct into the final product berberine or berberine salt, high-purity berberine or berberine salt can be obtained, the total impurity content is lower than 0.2%, the single impurity contentis lower than 0.1%, and the medicine safety is guaranteed.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a purification method and crystal form of berberine or a salt thereof. Background technique [0002] Berberine is an important alkaloid, which has been used in traditional Chinese medicine for a long time in our country. It can be extracted from plants such as Coptis chinensis, Cortex Phellodendri, and three needles. It has a significant antibacterial effect. Commonly used berberine hydrochloride is also called berberine hydrochloride, and its chemical structure is shown in formula I, and berberine can also exist in the form of sulfate. Berberine can resist pathogenic microorganisms, and has inhibitory effects on a variety of bacteria such as Shigella, Mycobacterium tuberculosis, Pneumococcus, Salmonella typhi and Diphtheria bacillus. Among them, it has the strongest effect on Shigella, and is often used to treat bacillary gastroenteritis and dysentery. a...

Claims

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Application Information

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IPC IPC(8): C07D455/03
CPCC07B2200/13C07D455/03
Inventor 谢永居赵宗敏郑裕义胡露伟卓晨万风云吴德冬
Owner JIANGXI FUSHINE PHARMA CO LTD
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