Purification method and crystal form of berberine or its salt

A purification method and technology for berberine, applied in the field of purification of berberine or its salt, can solve the problems of low efficiency, inability to meet standards, low success rate and the like, and achieve the effects of simple operation, mild reaction conditions and guaranteed safety.

Active Publication Date: 2021-09-17
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 its salt
  • Purification method and crystal form of berberine or its salt
  • Purification method and crystal form of berberine or its salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] 38.3 g of berberine sulfate (0.10 mmol, 87% purity) were dissolved in 2.0 L of water to give a brown solution, and 0.10 L of 1N aqueous sodium hydroxide solution was added at room temperature. After stirring at room temperature, 0.01 liter (small amount) of acetone was added dropwise. After the light yellow crystals were precipitated, stirring was continued for 2 hours, and the light yellow berberine acetone adduct was obtained by filtration. The single crystal structural formula of the obtained acetone adduct is as follows figure 1 shown (single crystal analysis using a 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 pattern of the obtained acetone adduct is shown in figure 2 (Performed using a Bruker D8 diffractometer, available from Bruker AXS Inc TM (Madison, Wisconsin), assayed by mounting the sample (approximately 10 mg) on ​​a single crystal si...

Embodiment 2

[0090] 32 g of berberine hydrochloride (purity of 90%) and 1280 ml of methanol were added dropwise with 428 ml of 0.2N NaOH at about 20° C. to obtain a brown clear liquid. After the dropping was completed, the mixture was stirred for 10 min and filtered, and 172 ml of acetone was added dropwise to the filtrate. After dripping, the temperature was lowered to 10-15 °C, stirred for 2 h, filtered, and dried at room temperature to obtain berberine acetone complex. The XRD data were consistent with figure 2 Basically the same. Put the whole batch of wet products and 1600ml of water into a 2000ml bottle, and add 160ml of 1mol / L hydrochloric acid dropwise. After dripping, the temperature was raised to 80-100°C to obtain a yellow liquid and kept for 10min. 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, and dried by suction, namely 27.2g of berb...

Embodiment 3

[0092] Utilize 86% berberine acetate to replace "38.3 grams of berberine sulfate" in Example 1, the molar weight is the same, carry out the same reaction, and finally the yield of berberine hydrochloride obtained is 85%, purity 99.85 %, and the single impurity content is lower than 0.1%.

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Abstract

The invention discloses a method for purifying berberine or its salt, comprising: converting a raw material mainly containing berberine or berberine salt I into an acetone adduct of berberine, and then 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 adduct crystal form of berberine. Adopt purification method of the present invention, berberine acetone adduct is converted into berberine acetone adduct by raw material containing berberine or berberine salt, then berberine acetone adduct is converted into final product berberine or its salt, can obtain high The pure berberine or its salt has a total impurity content of less than 0.2 percent and a single impurity content of less than 0.1 percent, which ensures the safety of the drug.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and particularly relates to a purification method and crystal form of berberine or a salt thereof. Background technique [0002] Berberine is an important alkaloid and a traditional Chinese medicine that has been used for a long time in my country. It can be extracted from plants such as Coptis chinensis, Treats, and three needles. It has significant bacteriostatic effect. The 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 fight against pathogenic microorganisms and has inhibitory effects on a variety of bacteria such as Shigella, Mycobacterium tuberculosis, Pneumococcus, Typhoid Bacillus and Diphtheria Bacillus, among which it has the strongest effect on Shigella, and is often used to treat bacterial gastroenteritis, dysentery and other ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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