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Technique for preparing berberine hydrochloride by microwave-enzyme method

A technology for the preparation of berberine hydrochloride and enzymatic method, applied in the direction of organic chemistry, etc., can solve the problems of low purity of berberine hydrochloride, inability to realize large-scale production, large consumption of organic solvents, etc., achieve wide application range, improve clarity, highly selective effect

Inactive Publication Date: 2013-12-11
NANJING TONGZE AGRI SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ubiquitous shortcomings such as high cost, large consumption of organic solvents, poor selectivity, low purity of berberine hydrochloride and inability to realize large-scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Grind the three needle medicinal materials and pass through a 30-mesh sieve to obtain a coarse powder; put the above coarse powder into a sulfuric acid solution with a pH value of 3, the solid-to-liquid ratio is 1:15, and then add 0.8% of the weight of the coarse powder to it. Cellulase, enzymatic hydrolysis at 50°C for 2 hours; put the converted material in a microwave extractor with a microwave power of 200W and an extraction time of 1 minute; add milk of lime to the extract to adjust the pH value 9, put it in a water bath, treat at 75°C for 10 minutes, filter out the precipitate, and obtain the filtrate; use 8% hydrochloric acid to adjust the pH of the filtrate to 2, add 5% NaCl in the volume of the filtrate, stir to dissolve, and let it stand , to obtain a yellow precipitate, washed with water, dried, heated to dissolve with absolute ethanol and recrystallized 3 times to obtain a berberine hydrochloride product.

Embodiment 2

[0020] Grind the three needle medicinal materials and pass through a 30-mesh sieve to obtain a coarse powder; put the above coarse powder into a sulfuric acid solution with a pH value of 4, with a solid-to-liquid ratio of 1:18, and then add 0.6% of the weight of the coarse powder to it. Cellulase, enzymatic hydrolysis at 55°C for 3 hours; put the converted material in a microwave extractor with a microwave power of 350W and an extraction time of 2 minutes; add milk of lime to the extract to adjust the pH value to 10, put it in a water bath, treat at 80°C for 10 minutes, filter out the precipitate, and obtain the filtrate; then use 8% hydrochloric acid to adjust the pH of the filtrate to 3, add 7% NaCl in the volume of the filtrate, stir to dissolve, and let it stand , to obtain a yellow precipitate, washed with water, dried, heated to dissolve with absolute ethanol and recrystallized 3 times to obtain a berberine hydrochloride product.

Embodiment 3

[0022] Grind the three needle medicinal materials and pass through a 30-mesh sieve to obtain a coarse powder; put the above coarse powder into a hydrochloric acid solution with a pH value of 5, the solid-to-liquid ratio is 1:20, and then add 0.3% of the weight of the coarse powder to it. Cellulase, enzymatic hydrolysis at 60°C for 4 hours; put the converted material in a microwave extractor with a microwave power of 400W and an extraction time of 3 minutes; add milk of lime to the extract to adjust the pH value to 9.5, put it in a water bath, treat at 85°C for 10 minutes, filter out the precipitate, and obtain the filtrate; then use 8% hydrochloric acid to adjust the pH of the filtrate to 4, add 8% NaCl of the filtrate volume, stir to dissolve, and let it stand , to obtain a yellow precipitate, washed with water, dried, heated with methanol to dissolve and recrystallized three times to obtain berberine hydrochloride product.

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PUM

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Abstract

The invention relates to a technique for preparing berberine hydrochloride by a microwave-enzyme method, which comprises the following steps: a. pulverization and screening of berberis root; b. acidic cellulase enzymolysis; c. microwave-assisted extraction; d. high-temperature and adjusted pH inactivation; and e. near-saturation precipitation of berberine hydrochloride with diluted acid and sodium chloride. The berberis root is used as the raw material, thereby fully utilizing the cellulase to destroy the cell walls of the plant; and the cavitation of ultrasonic is utilized to increase the molecular motion frequency and speed of the substance and enhance the penetrating power of the solvent, thereby enhancing the leaching speed and leaching frequency of the effective component, and further enhancing the leaching rate of berberine. The invention has the advantages of simple technique, mild reaction conditions, high selectivity, short extraction time and the like, and maximizes the extraction yield.

Description

technical field [0001] The invention belongs to the field of natural organic chemistry, and relates to a method for preparing berberine hydrochloride, in particular to a method for preparing berberine hydrochloride by using microwave combined with an enzyme method. Background technique [0002] The three needles are the dried roots of various plants belonging to the same family of Berberidaceae, also known as copper acupuncture, Coptis thorn, Coptis chinensis, Xiaohuanglian, Phellodendron punctatus, Berberis, etc. It is widely distributed throughout the country and is a commonly used Chinese herbal medicine. It is often used to replace Cortex Phellodendron and Coptis chinensis for medicinal purposes, with a wide range of treatments and definite curative effects. The three needle rhizomes contain a variety of isoquinoline alkaloids, which are the main components. They have the functions of antibacterial and anti-inflammatory, clearing away heat and detoxification, lowering bl...

Claims

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Application Information

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IPC IPC(8): C07D455/03
Inventor 杨存
Owner NANJING TONGZE AGRI SCI & TECH
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