SU1123700A1 - Method of obtaining iodide berberine - Google Patents

Abstract

A method for producing berberin iodide by extracting a Berberis oblonga plant with ethanol followed by thickening of the extract and precipitating the target product with an alkali metal iodide, characterized in that, in order to increase the yield of the target product, young shoots of Berberis oblonga are used as a source of raw material, and they are used as a source of blended chambers by combining the mixture with a mixture of blended chambers and alkaline metal iodide. water, filtering and alkalizing with ammonia, extract the tertiary alkaloids with ether, then the mother liquor is acidified and berberine iodide is precipitated by adding an aqueous solution. KJ.

Description

The invention relates to the pharmaceutical industry, namely, the production of berberine iodide, which is a raw material for the preparation of canadine, as well as berberine bisulfate.

A method is known for producing berberine iodide from the bark and wood of the roots of Berberis oblonga by extraction with ethanol, followed by concentration of the extract and precipitation of the target product by the addition of NaJ 1.

The disadvantages of this method are the low yield of the target product, as well as the fact that harvesting the roots leads to the destruction of large stocks of Berberis oblonga.

The purpose of the invention is to increase the yield of the target product.

This goal is achieved in that according to the method of producing berberine iodide by extracting the plant Berberis oblonga with ethanol followed by thickening the extract and precipitating the target product with alkali metal iodide, young shoots of Berberis oblonga are used as a source of raw material, from the thickened extract of which after diluting with water, filtering and underlaying the water after filtering it and adding it. the tertiary alkaloids are extracted with ammonia with ether, then the mother liquor is acidified and berberine iodide is precipitated by adding an aqueous solution of the short-circuit.

Example, kg of crushed young shoots of Berberis oblonga are percolated with ethanol (3 liters) to a negative reaction to alkaloids. The ethanolic extract is evaporated to a thick mass, the residue is diluted with 0.5 l of water, triturated and filtered. The clear filtrate is basked with 25% to pH 9-10. Alkaloids are extracted with ether 5 times in 200 ml each. The combined ether extracts are evaporated. 2.5 g of ether are obtained. Then alkaloids are extracted from the alkaline solution with chloroform 5 times in 200 ml each, and 0.95 g of the total of alkaloids is obtained. After this, the alkaline solution is acidified with concentrated HC1 to pH 1 and a 50% aqueous solution of CG, 50 ml, is added in portions. This gives a yellow amorphous precipitate of technical berberine iodide (2.5 g), which is recrystallized from hot methanol and dried at 60-70 °.

Chromatographic control of the obtained technical product on a silica gel plate in the systems chloroform - methanol (9: 1), toluene - acetone - methanol - ammonia (41.5: 49: 5: 4), methanol-ammonia-water (8: 1: 1 ) shows that the latter contains mainly berberine iodide, with the exception of minor impurities.

During the recrystallization of 2.5 g of the technical product from hot methanol, 2.2 g of chromatographically pure berberine iodide was obtained, the purity of the preparation was checked by comparison with a genuine sample.

The table presents the data on the yield of berberine iodide when it is obtained by the proposed method and the prototype method type.

The proposed method provides an exhaustive isolation of berberine iodide from the plant extract. The latter is precipitated after prior removal of the accompanying extractives, which facilitates its further purification. The loss of berberine iodide is minimized. The yield of pure berberine iodide is 88% of the weight of the technical product, and the loss is 12 / o (according to the prototype method, 69.2% of the weight of the technical product). The proposed type of raw material - young shoots of Berberis oblonga is renewed annually and contains 0.22 / o berberine. Thus, the proposed method also provides for the expansion of the raw material base for the production of berberine iodide.

Claims (1)

METHOD FOR PRODUCING BERBERIN IODIDE by extracting the Berberis oblonga plant with ethanol, followed by thickening the extract and precipitating the target product with alkali metal iodide, characterized in that, in order to increase the yield of the target product, young shoots of Berberis oblonga are used as a source of raw material, from the condensed extract of which after dilution with water, filtration and alkalization with ammonia, tertiary alkaloids are extracted with ether, then the mother liquor is acidified and berberine iodide precipitated by adding an aqueous solution. KJ.