Method for separating carnosic acid from rosemary leaf extract

A technology of rosemary leaf extraction and carnosic acid, applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problems of poor thermal stability, low efficiency, easy oxidation, etc., and achieve antioxidant activity Good, improve economic efficiency, and shorten the column passing time

Active Publication Date: 2011-07-06
湖南和广生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are mainly the following difficulties in the research on the separation of carnosic acid at home and abroad: 1. Carnosic acid has poor stability in many solvents and is easily oxidized. It is almost impossible to obtain high-content products by solvent separation methods; 2. Ordinary silica gel column Chromatographic methods take a long time to separate carnosic acid, and the outflow of carnosic acid components is slow and the efficiency is low; 3. Most of the subsequent steps of separation include recrystallization process, carnosic acid not only has poor solvent stability, but also has poor thermal stability The same is not good; 4. The cost is high and there is no actual economic benefit

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The method for isolating carnosic acid from rosemary leaf extract comprises the following steps:

[0024] (1) Add 200ml of absolute ethanol and 2.5ml of phosphoric acid into a 500ml round bottom flask to make a phosphoric acid-ethanol solution, weigh 100 grams of column chromatography silica gel and disperse it in the phosphoric acid-ethanol solution, and vacuum for 15 minutes to remove the silica gel The air between the particles prevents carnosic acid from being oxidized during the process of passing through the column, then ultrasonically infiltrates for 20 minutes, puts it in a rotary evaporator to recover ethanol, and dries at 120°C for 8 hours to obtain a phosphoric acid-silica gel stationary phase, which is ready for use;

[0025] (2) Take 2 grams of rosemary leaf extract containing 60% carnosic acid, be dissolved in ethyl acetate, add 10 grams of phosphoric acid-silica gel stationary phase, fully stir, and reclaim ethyl acetate in a rotary evaporator, Obtain the...

Embodiment 2

[0031] The method for isolating carnosic acid from rosemary leaf extract comprises the following steps:

[0032] (1) Add 200ml of absolute ethanol and 5ml of phosphoric acid into a 500ml round bottom flask to make a phosphoric acid-ethanol solution, weigh 100 grams of column chromatography silica gel and disperse it in the phosphoric acid-ethanol solution, and vacuumize for 15 minutes to remove silica gel particles The air between them was used to prevent the carnosic acid from being oxidized during the process of passing through the column, and then ultrasonically infiltrated for 20 minutes, then placed in a rotary evaporator to recover ethanol, and dried at 120°C for 8 hours to obtain a phosphoric acid-silica gel stationary phase, which is ready for use;

[0033] (2) Take 2 grams of rosemary leaf extract containing 60% carnosic acid, be dissolved in ethyl acetate, add 10 grams of phosphoric acid-silica gel stationary phase, fully stir, and reclaim ethyl acetate in a rotary ev...

Embodiment 3

[0039] The method for isolating carnosic acid from rosemary leaf extract comprises the following steps:

[0040] (1) Add 200ml of absolute ethanol and 7.5ml of phosphoric acid into a 500ml round bottom flask to make a phosphoric acid-ethanol solution, weigh 100 grams of column chromatography silica gel and disperse it in the phosphoric acid-ethanol solution, and vacuum for 15 minutes to remove the silica gel The air between the particles prevents carnosic acid from being oxidized during the process of passing through the column, then ultrasonically infiltrates for 20 minutes, puts it in a rotary evaporator to recover ethanol, and dries at 120°C for 8 hours to obtain a phosphoric acid-silica gel stationary phase, which is ready for use;

[0041] (2) Take 2 grams of rosemary leaf extract containing 60% carnosic acid, be dissolved in ethyl acetate, add 10 grams of phosphoric acid-silica gel stationary phase, fully stir, and reclaim ethyl acetate in a rotary evaporator, Obtain the...

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PUM

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Abstract

The invention discloses a method for separating carnosic acid from a rosemary leaf extract. The method comprises the following steps of: dispersing column chromatography silica gel in a phosphoric acid-ethanol solution, vacuumizing, ultrasonically soaking, recycling ethanol and drying to obtain a phosphoric acid-silica gel stationary phase; filling the phosphoric acid-silica gel stationary phase into a chromatography column tube, imported with high-purity nitrogen for protection, to obtain a phosphoric acid-silica gel chromatography column; and dissolving the rosemary leaf extract in ethyl acetate, adding the phosphoric acid-silica gel stationary phase into the mixture, fully stirring to recycle the ethyl acetate to obtain a stationary phase adsorbing the rosemary leaf extract, adding thestationary phase adsorbing the rosemary leaf extract into the phosphoric acid-silica gel chromatography column, eluting, collecting fractions and performing vacuum drying to obtain carnosic acid. By adopting the method, the carnosic acid is separated independently only by once column chromatography, the column chromatography time is short, the purity is up to 92 percent, and the application of a product in the market is promoted.

Description

technical field [0001] The invention relates to a method for separating carnosic acid from rosemary leaf extract. Background technique [0002] Rosemary (Rosmarinus offoconalis L.) is a plant of the genus Rosmarinus of the Lamiaceae, rich in a variety of efficient and safe antioxidant components. Rosemary extract is a new type of excellent natural antioxidant, which can effectively remove free radicals in the body, prevent food from deteriorating, and has anti-inflammatory, anti-tumor, and anti-HIV effects ([1] Yang Yan. Rosemary Extract Properties and applications of substances [J]. China Food Industry, 1999, (3): 38-39. [2] OffordEA, MacéK, Avanti O, et al. Cancer Letters [J]. 1997, 114 (12): 275 -281.). Carnosic acid (CA) is the most important active ingredient in rosemary fat-soluble antioxidants. It not only has antioxidant activity, but also has anticancer properties. It is widely used in cosmetics, medicines and health products. [0003] At present, there are mainl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C62/34C07C51/42
Inventor 曾健青左雄军粱钰陈瞾
Owner 湖南和广生物科技有限公司
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