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Preparation and detection method of salvianolic acid B from salvia miltiorrhiza

A technology of salvianolic acid and salvia miltiorrhiza is applied in the field of preparation of salvianolic acid B of salvia miltiorrhiza. The effect of high rate and high content

Active Publication Date: 2009-05-20
PHARMA RES INST OF BENCAO TIANYUAN OF BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The literature "Research on the preparation process of high-purity salvianolic acid B (Shi Zhen Guoyue Guoyao 2005, Volume 16, Issue 6, 476-478, Wang Fengmei, etc.)" adopts the methods of water extraction, ethyl acetate extraction, and macroporous resin purification. Obtain 91.8% of salvianolic acid B; literature "Screening research on the separation of salvianolic acid B by macroporous resin (Shizhen Guoyi Guoyao, Volume 17, No. 6, 2006, 973-974, Ye Yong)", using alcohol extraction, The method of macroporous adsorption resin, obtains salvianolic acid B; The analysis method that above-mentioned document adopts is: the detection and analysis method of isocratic mobile phase, the scientificity of this analysis method is open to question, and the content of its salvianolic acid B is not The content of the real substance, and the extraction rate of the above-mentioned side is not high, needs further research; Chinese patent CN1488627A "preparation method of salvianolic acid B magnesium salt" adopts ethanol extraction, macroporous adsorption resin method, polyamide chromatography, and the obtained content is greater than 90% salvianolic acid B, although this method can obtain a certain content of salvianolic acid B, but the detection method of its content is not clear, and the reliability of the results needs to be studied

Method used

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  • Preparation and detection method of salvianolic acid B from salvia miltiorrhiza
  • Preparation and detection method of salvianolic acid B from salvia miltiorrhiza
  • Preparation and detection method of salvianolic acid B from salvia miltiorrhiza

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Embodiment 1

[0056] Take 1 kg of Salvia miltiorrhiza, extract with ethanol, filter, combine the filtrates, concentrate, centrifuge, take the supernatant and pass it through a HPD-100 macroporous adsorption resin column, wash and discard with water, elute with 10% ethanol, collect the eluate, and concentrate to ethanol to the end, centrifuge, take the supernatant and pass it through a polyamide adsorption resin column, wash and discard with water, elute with 30% ethanol, discard the eluate, elute with 50% ethanol, collect the eluate and concentrate until ethanol is exhausted, the concentrated solution Adjust the pH value to 1, extract with the organic solvent n-butanol, concentrate the organic phase, and dry in vacuum to obtain 32.7 g of salvianolic acid B of the present invention.

Embodiment 2

[0058] Take 10kg of Salvia miltiorrhiza, extract with ethanol, filter, combine the filtrates, concentrate, centrifuge, take the supernatant and pass it through HPD-100A macroporous adsorption resin column, wash and discard with water, elute with 20% ethanol, collect the eluate, and concentrate to ethanol To the end, centrifuge, take the supernatant and pass it through a polyamide adsorption resin column, wash and discard with water, elute with 50% ethanol, discard the eluate, elute with 70% ethanol, collect the eluate and concentrate to ethanol to the end, the concentrated solution Adjust the pH value to 4, extract with organic solvent propyl acetate, concentrate the organic phase, and dry in vacuum to obtain 14.4 g of salvianolic acid B3 of the present invention.

Embodiment 3

[0060] Take 1 kg of Salvia miltiorrhiza, extract with ethanol, filter, combine the filtrates, concentrate, centrifuge, take the supernatant, pass through 1400, wash and discard, elute with 15% ethanol, collect the eluate, concentrate until the ethanol is exhausted, centrifuge, and take the upper The supernatant was passed through a polyamide adsorption resin column, washed with water and discarded, 40% ethanol was eluted, the eluent was discarded, and 60% ethanol was eluted, the collected eluate was concentrated to ethanol to the end, and the concentrated solution was adjusted to pH 2.5 with The organic solvent was extracted with ethyl acetate, the organic phase was concentrated, and dried in vacuum to obtain 34.9 g of salvianolic acid B of the present invention.

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Abstract

The invention discloses a preparation method and an inspection method of salvianolic acid B of salvia miltiorrhiza, which is characterized in that the salvianolic acid B of the of salvia miltiorrhiza is obtained by a macroporous adsorptive resin method, a polyamide adsorptive resin method and an organic solvent extraction method after the salivae miltiorrhizae is extracted by ethanol; the content of the prepared salvianolic acid B of the salvia miltiorrhiza is more than or equal to 90 percent and less than 100 percent by adopting a scientific inspection and analysis method of a gradient mobile phase; the preparation method has good extraction ratio and high purification and is simple and easy for industrialized production; the inspection and analysis method has good resolution and accurate analysis result.

Description

technical field [0001] The invention relates to the technical field of traditional Chinese medicine, in particular to a preparation method and a detection and analysis method of salvianolic acid B, and further relates to a preparation method and a detection and analysis method of salvianolic acid B with a content greater than or equal to 90%. Background technique [0002] The ingredients contained in Danshen include: ineffective ingredients such as polysaccharides, proteins, and tannins, and effective ingredients such as water-soluble and fat-soluble ingredients. Among the active ingredients, fat-soluble ingredients mainly include tanshinones and rosolitazones, and most tanshinones are diterpene compounds. Most of them are diterpene quinone compounds. The water-soluble components of Salvia miltiorrhiza have a phenolic acid structure, collectively called salvianolic acid, including danshensu, salvianolic acid A, B, C, D, E, H, I, J, Salvianolic acid C, rosmarinic acid, shikon...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/80
Inventor 顾群李志刚渠守峰米长江姜威阮爱华
Owner PHARMA RES INST OF BENCAO TIANYUAN OF BEIJING
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