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Preparation process of rosmarinic acid

A technology of rosmarinic acid and preparation process, applied in the separation/purification of carboxylate, organic chemistry and other directions, can solve the problems of large amount of ethanol, low product purity, low extraction rate and the like

Inactive Publication Date: 2010-10-20
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, domestic and foreign studies on rosmarinic acid have shown that it has important application value in medicine, food, and cosmetics. Therefore, many studies have been carried out on the extraction of rosmarinic acid. For example, patent 200710017142.9 discloses "a perilla leaf The method for preparing rosmarinic acid” uses citric acid extraction, macroporous resin adsorption and concentration under reduced pressure. , acid adjustment, resin column chromatography, and crystallization methods, which use a large amount of solvent and have not been decolorized; "Experimental Research on the Optimization of Ethanol Extraction of Rosmarinic Acid in Perilla" published by Zhou Pingping, which uses 50% Ethanol extraction, large amount of ethanol and low extraction rate

Method used

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  • Preparation process of rosmarinic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0025] After crushing 20kg of Prunella vulgaris, soak in 240L of water at 60°C for 4 hours, then ultrasonically extract for 30 minutes, filter, add 60L of 15% ethanol to the filter residue for reflux extraction for 1 hour, filter, combine the two filtrates, add 560g of sodium metabisulfite, and then add Equal amount of 004×7 strong acidic cation exchange resin, stir while adding, let stand for 1 hour, filter and concentrate to 1 / 10 of the original volume, take 15 times the amount of 120-200 mesh neutral alumina column, add the concentrated solution to the column Adsorption, sequentially measure 2BV petroleum ether, 7BV ethyl acetate, 3BV30% ethanol, 2BV80% ethanol to elute, collect rosmarinic acid fraction, then add 5% activated carbon and indirectly heat to 60°C, stir for 30 minutes, and pump while hot Filtrate, then add 2% diatomaceous earth, heat to 50°C, stir and absorb for 30 minutes, filter and concentrate through KJ-NSRO-30 (4040) nanofiltration membrane, recover reagent...

Embodiment 2

[0027] After crushing 50kg of Eupatorium, soak in 750L of water at 55°C for 5 hours, then ultrasonically extract for 20 minutes, filter, add 200L of 30% ethanol to the filter residue for reflux extraction for 0.5 hours, filter, combine the two filtrates, add 450g of hydrogen peroxide, and then Add the same amount of D113 macroporous cation exchange resin, stir while adding, let it stand for 4 hours, filter and concentrate to 1 / 15 of the original volume, take 18 times the amount of pretreated XAD-761 macroporous resin to pack, add the concentrated solution Column adsorption, sequentially measure 2BV petroleum ether, 6BV ethyl acetate, 4BV30% ethanol, 2BV80% ethanol to elute, collect rosemarinic acid fraction, then add 2% activated carbon and indirect heat to 60 ° C, stir for 45 minutes, while hot Suction filtration, then add 1% diatomaceous earth, heat to 40°C, stir and absorb for 30 minutes, filter and concentrate through KJ-NSRO-30 (4040) nanofiltration membrane, recover the r...

Embodiment 3

[0029] Crush 50kg of mint and soak in 700L of water at 80°C for 3 hours, then ultrasonically extract for 45 minutes, filter, add 150L of 50% ethanol to the filter residue for reflux extraction for 2 hours, filter, combine the two filtrates, add 800g of sodium metabisulfite, and then add Measure 001×7 strong acidic cation exchange resin, stir while adding, let stand for 3 hours, filter and concentrate to 1 / 12 of the original volume, take 15 times the amount of pretreated HPD400 macroporous resin, and add the concentrated solution to the column for adsorption , sequentially measure 3BV petroleum ether, 5BV ethyl acetate, 5BV30% ethanol, 2BV80% ethanol to elute, collect the rosmarinic acid fraction, then add 5% activated carbon and indirectly heat to 60°C, stir for 60 minutes, and suction filter while hot , then add 1% diatomaceous earth, heat to 50°C, stir and adsorb for 30 minutes, filter and concentrate through KJ-NSRO-30 (4040) nanofiltration membrane, recover the reagent, add...

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Abstract

The invention relates to a preparation process of rosmarinic acid, which adopts the following steps for preparing the rosmarinic acid: combining aqueous extraction and ethanol extraction, carrying out ion exchange, placing materials on a chromatographic separation medium for gradient elution, and carrying out secondary decolourization, nanofiltration membrane concentration and recrystallization. The method solves the problems of large extraction solvent amount, much chemical residual, poor color intensity and low extraction rate. Products produced by adopting the method have the advantages of good quality, high purity, high extraction rate, simple operation and convenient scale production.

Description

Technical field: [0001] The invention relates to a preparation process of rosmarinic acid, in particular to a method of combining water extraction and alcohol extraction, ion exchange, chromatographic separation, secondary decolorization and recrystallization. Background technique: [0002] Rosmarinic acid is a phenolic acid compound. [0003] Molecular formula: C 18 h 16 o 8 ;Molecular weight: 360.33 [0004] Chemical name: [R(E)]α-{[3-(3,4-dihydroxyphenyl)-1-oxo-2-propenyl]oxy}-3,4-dihydroxyphenylpropionic acid [0005] Chemical Structure: [0006] [0007] Physical and chemical properties: Rosmarinic acid is light yellow powder, mp192-195℃. [0008] Rosmarinic acid is widely distributed in plants, and mainly exists in labiatae plants such as rosemary, perilla leaves, and salvia miltiorrhiza. As an antioxidant, rosmarinic acid has a strong activity of scavenging free radicals in the body and antioxidant effect, and its antioxidant activity is stronger than that o...

Claims

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Application Information

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IPC IPC(8): C07C69/732C07C67/48
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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