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Method for simultaneously preparing high-purity carnosol and carnosic acid from rosemary

A technology of carnosol and carnosic acid is applied in the separation field of SephadexLH-20 gel column chromatography, which can solve the problems of waste, loss, resource waste and the like, and achieve the effect of simple and easy operation.

Active Publication Date: 2018-07-13
BEIJING UNION UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the prior art, there is only the method for preparing a single high-purity carnosic acid with rosemary or its extract, or the method for a single carnosol, and there is no method for obtaining two high-purity components at the same time. At the same time, it causes the waste and loss of another ingredient, which causes a lot of waste of resources in industrialized mass production

Method used

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  • Method for simultaneously preparing high-purity carnosol and carnosic acid from rosemary
  • Method for simultaneously preparing high-purity carnosol and carnosic acid from rosemary
  • Method for simultaneously preparing high-purity carnosol and carnosic acid from rosemary

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1 prepares rosemary extract

[0022] 10Kg of dried rosemary leaves were crushed through a 20-mesh sieve, and the solvent was ultrasonically extracted with 60% ethanol aqueous solution at a liquid-to-solid ratio of 12:1 (L / Kg) for 75 minutes. Continuous extraction was performed three times, the extracts were combined, concentrated under reduced pressure and evaporated to dryness to obtain the rosemary extract, wherein the content of carnosol was 10.28wt%, and the content of carnosic acid was 17.47wt%.

Embodiment 2

[0023] Example 2 Simultaneous preparation of high-purity carnosol and carnosic acid from rosemary extract

[0024] (1) Normal phase silica gel column separation and purification

[0025] Rosemary extract 500g prepared in Example 1 was added in 5000ml water-saturated ethyl acetate, ultrasonically dissolved for 0.5 hour, filtered, and insolubles were removed. The filtrate was mixed with 500 g of normal phase silica gel (160-200 mesh), and 3000 g of normal phase silica gel (160-200 mesh) was dry-loaded to the column, and purified by normal pressure normal phase silica gel column chromatography. Carry out gradient elution, according to the order of elution, each mobile phase and extract are as follows:

[0026] (1) The mobile phase is chloroform, the elution volume is 5L, and the elution components are mainly small polar impurities;

[0027] (2) The mobile phase is chloroform, methanol, acetic acid, the volume ratio is 100:0:1‰, the elution volume is 10L, and the main component ...

Embodiment 3

[0056] Example 3 Simultaneous preparation of high-purity carnosol and carnosic acid from rosemary extract

[0057] (1) Normal phase silica gel column separation and purification

[0058] The same method as in step (1) of Example 2 was used to obtain carnosol components with a content of about 85% and carnosic acid with a content of about 90%.

[0059] (2) Gel column separation and purification

[0060] The carnosol fraction containing about 85 wt% obtained in step (1) was repeatedly purified with hydroxypropyl dextran gel (Sephadex LH-20 gel). The length of the gel column is 120cm, the column is packed by wet method, and the sample is loaded by wet method. The mobile phase was eluted with chloroform:methanol=2:1 (volume ratio), the flow rate of the mobile phase was 3ml / min, and the chromatography time was 500min. The same components were combined and evaporated to dryness under reduced pressure to obtain 40.8 g of carnosol with a high content of ≥98%.

[0061] Using the ab...

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Abstract

The invention relates to a method for simultaneously preparing high-purity carnosol and carnosic acid from rosemary. The method comprises the steps of extracting the flowers and leaves of the rosemarywith an ethanol aqueous solution to obtain a rosemary extract, and dissolving the extract in water saturated ethyl acetate; separating the obtained solution with positive phase silica gel, carrying out gradient elution according to a ratio of chloroform to methanol to acetic acid being equal to (100-95) to (0-5) to (0-0.001), merging the same components, and carrying out vacuum concentration to obtain crude products of the carnosol and the carnosic acid; then, separately carrying out Sephadex LH-20 gel column chromatography purification on the crude products, eluting a mobile phase with chloroform-methanol or petroleum ether-chloroform-methanol, merging the same components, and drying by distillation under the reduced pressure to obtain the carnosol and the carnosic acid which have the purities of 98% or above. The method can be used for simultaneously preparing the high-purity carnosol and carnosic acid from the rosemary. A gel column can be repeatedly used, and column chromatographyis short in time and high in efficiency. The method is simple, easy to operate and high in yield, thus being suitable for large-scale production.

Description

technical field [0001] The invention relates to a method for simultaneously preparing high-purity natural antioxidant active ingredients carnosol and carnosic acid from rosemary, in particular to a method that has a significant separation effect on the separation of a large amount of carnosol and carnosic acid Sephadex LH-20 gel column chromatography separation method. Background technique [0002] Rosemary is a natural antioxidant, and carnosol and carnosic acid are its main antioxidant components. With the rapid development of the functional food industry, the demand for edible antioxidant products is increasing; And along with the successful introduction of rosemary to my country and its large-scale cultivation, finding a simple and cheap method for preparing high-purity antioxidant active monomers from rosemary or its extract will have good use value and Practical significance. [0003] Many patents have reported the extraction method of antioxidant active substances in ...

Claims

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Application Information

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IPC IPC(8): C07C51/42C07C51/47C07C62/32C07D493/08
CPCC07C51/42C07C51/47C07D493/08C07C62/32
Inventor 李金杰尚小雅冀麟麟栾娜王欣郭俊霞
Owner BEIJING UNION UNIVERSITY
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