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Purification method of berberine or its hydrochloride

A purification method and technology of berberine, which is applied in the field of purification of berberine or its hydrochloride, can solve the problems of failure to meet standards, low efficiency, low success rate, etc., and achieve the effects of mild reaction conditions, simple and convenient operation, and guaranteed safety

Active Publication Date: 2021-05-25
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 of berberine or its hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1: acesulfame potassium salt method

[0036] 9.09 grams of berberine hydrochloride (purity 95%) was heated to 80 degrees and dissolved in 75 milliliters of water, and stirred for 30 minutes to obtain an orange solution. At the same time, 5.44 grams of acesulfame potassium was dissolved in water and added to the above solution, stirred for 10 minutes, and precipitates were precipitated, cooled to 25 degrees, and continued to stir and crystallize for 16 hours. Filter, the filtered solid is suspended in 30 ml of water, add 1N HCl aqueous solution (27 mmol), stir and heat up to 90 degrees, after 2 hours, cool down to about 10 degrees, continue stirring for 2 hours, filter and dry to obtain 8.5 grams of berberine hydrochloride . The purity is 99.85%, and the impurity content is less than 0.1%.

[0037] The NMR data of berberine hydrochloride are as follows:

[0038] 1 H-NMR, CD 3 OD, 400MHZ, δ3.28-3.31[m,2H], δ4.12[s,3H], δ4.23[s,3H], δ4.97-4.99[m,2H], δ6.14[...

Embodiment 2

[0039] Embodiment 2: saccharin sodium salt method

[0040] Add 14.88g of berberine hydrochloride (purity 96%) and 800ml of water to a 2L four-necked bottle at room temperature, heat up to 75°C to dissolve and keep stirring for 30min, then add 10.68g of saccharin sodium solution (dissolved in 200ml of water) dropwise, and there are crystals Precipitate, keep warm for half an hour after adding, then drop to room temperature and keep stirring overnight, then filter to obtain berberine saccharin salt. Add 600ml of water to the berberine saccharin salt, slowly add 44ml of 1mol / L hydrochloric acid dropwise at room temperature, heat and stir for 1.5 hours after the addition, then raise the temperature to 80°C and stir for 2 hours, then cool down to room temperature and stir for 2 hours, then filter to obtain berberine hydrochloride , the yield was 89%. The purity is 99.85%, and the impurity content is less than 0.1%.

Embodiment 3

[0041] Embodiment 3: acesulfame potassium salt method

[0042] 9.09 g of berberine hydrochloride (purity 90%) was heated to 75°C and dissolved in 75 ml of water, and stirred for 30 minutes to obtain an orange solution. At the same time, 8.10 grams of acesulfame potassium was dissolved in water and added to the above solution, stirred for 10 minutes, and precipitates were precipitated, cooled to 25 degrees, and continued to stir and crystallize for 16 hours. Filter, the filtered solid is suspended in 30 ml of water, add 1N HCl aqueous solution (27mmol), stir and heat up to 80°C, after 2 hours, cool down to about 10°C, continue stirring for 2h, filter and dry to obtain 8.7g of berberine hydrochloride . The purity is 99.85%, and the impurity content is less than 0.1%.

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Abstract

The invention discloses a method for purifying berberine or its hydrochloride, which comprises: mainly including the reaction of the starting material mainly containing berberine, berberine hydrochloride or berberine sulfate with salt II, and converting it into an intermediate salt of berberine, Finally, the intermediate salt of berberine is converted into berberine or its hydrochloride. The present invention converts the starting material mainly containing berberine, berberine hydrochloride or berberine sulfate into an intermediate salt of berberine, removes impurities, and then converts the intermediate salt of berberine into berberine or its hydrochloride, The final product has a total impurity content of less than 0.2% and a single impurity content of less than 0.1%, which further ensures the safety of the drug.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a method for purifying berberine or its hydrochloride. 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. and other gastrointestinal di...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D455/03
CPCC07D455/03
Inventor 谢永居郑裕义赵宗敏万风云吴德冬
Owner JIANGXI FUSHINE PHARMA CO LTD
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