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Method for preparing berberine through separation from berberis julianae schneid

A technology of three needles and berberine, applied in the direction of organic chemistry, can solve the problems of many chemical reagents and types, complicated steps, high extraction cost, and achieve the effects of low cost, high purity, and few separation and purification steps.

Inactive Publication Date: 2019-06-28
海南制药厂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The amount and types of chemical reagents used in this method are too many, the steps are cumbersome, and the extraction cost is still high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take 100 grams of dry three needle powder crushed to 10-20 mesh, add 1L of water, heat to boil, keep warm and reflux for 2 hours, filter out the water extract; add 600-800mL of water, heat to boil, keep warm and reflux for 2 hours, filter out the water extract; Repeated extraction for 4 to 5 times, combined with water to extract and filter the solution, concentrated under reduced pressure to near dryness, stirred and dissolved with an appropriate amount of methanol while hot, poured out, stirred and dissolved repeatedly for 3 to 4 times, combined methanol liquid, concentrated under reduced pressure to about 100 ~120mL, adjust the pH value of the solution to 1~2 with concentrated hydrochloric acid, put it in the refrigerator, and precipitate yellow crystals after 4~8 hours, filter, wash with cold water, and wash with a small amount of ethyl acetate to obtain 0.96 grams of berberine hydrochloride.

Embodiment 2

[0022] Take 300 grams of dry three needle powder crushed to 10-20 mesh, add 2L of water, heat to boil, keep warm and reflux for 2.5h, filter out the water extract; add 1.5L of water, heat to boil, keep warm and reflux for 2.5h, filter out the water extract; This method is repeatedly extracted 4 to 5 times, combined with water to extract and filter the solution, concentrated under reduced pressure to near dryness, stirred and dissolved with an appropriate amount of methanol while hot, poured out, stirred and dissolved repeatedly for 3 to 4 times, combined methanol liquid, concentrated under reduced pressure to about 300-400mL, adjust the pH value of the solution to 1-2 with concentrated hydrochloric acid while it is hot, put it in the refrigerator, and precipitate yellow crystals after 4-6 hours, filter, wash with cold water, and wash with a small amount of ethyl acetate to obtain 1.71 grams of berberine hydrochloride.

Embodiment 3

[0024] Take 5kg of dry three needle fragments crushed to 1-3mm thin slices, add 25L of water, heat to boiling, keep warm and reflux for 1.5h, filter out the water extract; add 15-20L of water, heat to boil, keep warm and reflux for 2h, filter out the water extract; This method is repeatedly extracted 4 to 5 times, combined with water to extract and filter the solution, concentrated under reduced pressure to near dryness, stirred and dissolved with an appropriate amount of methanol while hot, poured out, stirred and dissolved repeatedly for 3 to 4 times, combined methanol liquid, concentrated under reduced pressure to about 5-6L, use concentrated hydrochloric acid to adjust the pH value of the solution to 1-2, put it in the refrigerator, and precipitate yellow crystals after 6-8 hours, filter, wash with cold water, and wash with a small amount of ethyl acetate to obtain 33.1 grams of berberine hydrochloride.

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PUM

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Abstract

The invention discloses a method for preparing berberine through separation from berberis julianae schneid. The method for preparing the berberine hydrochloride through separation mainly comprises thesteps that the berberis julianae schneid is directly boiled in water for extraction, after pressure reduction concentration, methyl alcohol or ethyl alcohol is adopted for dissolution, after an alcoholic solution is filtered and concentrated, the solution is adjusted to be acid in pH, and berberine hydrochloride crystals are separated out through refrigeration. According to the method, using of acid, alkali and salt is reduced, the steps are simple, and the purity of the separated berberine hydrochloride is significantly improved.

Description

technical field [0001] The invention relates to the technical field of plant extracts, in particular to a method for separating and preparing berberine from three needles. Background technique [0002] Berberine, also known as berberine, exists in many plants of 4 families and 10 genera such as Berberidaceae. Berberine is a yellow needle-like crystal, and berberine can be separated from ether. Yellow needle-like crystals. The melting point is 145°C. Soluble in water, insoluble in benzene, ether and chloroform. Berberine is a quaternary ammonium alkaloid, and the solubility of its salts in water is relatively small, for example, hydrochloride is 1:500, and sulfate is 1:30. Berberine is treated with different alkalis to obtain three different forms of berberine: quaternary ammonium form, aldehyde form and alcohol form, among which the quaternary ammonium form is the most stable. [0003] Berberine is a commonly used clinical broad-spectrum antibacterial drug, mainly used fo...

Claims

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Application Information

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IPC IPC(8): C07D455/03
Inventor 蒲含林赖潜李秀峰
Owner 海南制药厂有限公司
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