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Method used for separating coumarin in natural perfume

A technology of natural spices and coumarin, which is applied in the direction of organic chemistry, can solve the problems of cumbersome process, high preparation cost, and inability to separate coumarin, and achieve simple process, low cost, safety and improved application range Effect

Inactive Publication Date: 2018-07-06
澳华达香精(广州)有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method adopted in this patent requires the use of DNA-solid phase support. The preparation and purification of DNA-solid phase support itself is a very complicated technology, the process is cumbersome, and the preparation cost is also high. In addition, this technology cannot realize non-essential oil products. Separation of mesocoumarin
[0005] At present, there are no domestic literature reports on the separation of coumarin from natural spices such as Maoxiang extract, Osmanthus osmanthus extract, Grain Raingrass extract, and black coumarin tincture. The spice industry has not yet met industrial production and has economic application value. separation method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Mix Maoxiang extract and 10% concentration ethanol solution in a mass ratio of 1:10, mechanically stir for 30 minutes and then let stand for 30 minutes, filter the solution with a 300-mesh filter screen, and collect the filtered clear liquid;

[0022] (2) the filtered clear liquid obtained in step (1) is passed through the AB-8 macroporous resin column for adsorption, and the channeling fluid is collected;

[0023] (3) Use aqueous solution, ethanol, ethyl acetate, and the mixed solvent that these solvents are mixed in a certain proportion to carry out gradient elution to the macroporous resin column that has adsorbed perfume in step (2), and carry out fragrance to eluent Beanin content detection, keep 1# and 4# two low coumarin elution fractions;

[0024] (4) Mix the channeling fluid obtained in step (2) with the 1# and 4# eluent components obtained in step (3), and concentrate under reduced pressure at a temperature of 65°C and a vacuum of 0.98Mpa to obtain the lea...

Embodiment 2

[0028] (1) Mix Grain Raingrass extract and 5% ethanol solution at a mass ratio of 1:15, mechanically stir for 30 minutes and then let stand for 30 minutes, filter the solution with a 300-mesh filter, and collect the filtrate;

[0029] (2) the filtered clear liquid obtained in step (1) is passed through the AB-8 macroporous resin column for adsorption, and the channeling fluid is collected;

[0030] (3) Use aqueous solution, ethanol, ethyl acetate, and the mixed solvent that these solvents are mixed in a certain proportion to carry out gradient elution to the macroporous resin column that has adsorbed perfume in step (2), and carry out fragrance to eluent Beanin content detection, keep 1# and 3# two low coumarin elution fractions;

[0031] (4) Mix the channeling fluid obtained in step (2) with the 1# and 3# eluent components obtained in step (3), and concentrate under reduced pressure at a temperature of 60°C and a vacuum of 0.98Mpa to obtain the leached paste;

[0032] (5) A...

Embodiment 3

[0035] (1) Mix the Medicinal Rhinoceros extract and 15% ethanol solution in a mass ratio of 1:20, mechanically stir for 40 minutes and then let stand for 60 minutes, filter the solution with a 300-mesh filter, and collect the filtrated liquid;

[0036] (2) The filtered clear liquid obtained in step (1) is adsorbed through the DA-201 macroporous resin column, and the channeling fluid is collected;

[0037] (3) Use aqueous solution, ethanol, ethyl acetate, and the mixed solvent that these solvents are mixed in a certain proportion to carry out gradient elution to the macroporous resin column that has adsorbed perfume in step (2), and carry out fragrance to eluent Beanin content detection, retaining 2#, 3# and 5# three low-coumarin elution fractions;

[0038] (4) Mix the channeling liquid obtained in step (2) with the 2#, 3# and 5# eluent components obtained in step (3), and concentrate under reduced pressure at a temperature of 55°C and a vacuum of 0.92Mpa , get the extract;

...

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Abstract

The invention provides a method used for separating coumarin in natural perfume. The method comprises following steps: a mixed solvent is adopted for dissolving of the natural perfume, filtering is carried out, an obtained filtrate is subjected to adsorption using a macroporous resin so as to obtain a solution, organic solvents are adopted for gradient elution, specified elution components are collected, the collected elution components are mixed with the solution, an obtained mixture is subjected to condensation, after condensation, a coumarin substitute compound is added at a certain ratio,and blending is carried out so as to obtain a finished product. The method is capable of separating coumarin in natural perfume such as sweetgrass rhizome extract, Melilotus officinalis extract, grainrains grass extract, and Tonka bean tincture, the coumarin content of the finished product is lower than 1<mu>g / g, product safety is increased greatly, application range is widened greatly, operationof the method is simple, cost is low, and the method is suitable for industrialized production.

Description

technical field [0001] The invention relates to a process for separating coumarin from natural spices, belonging to the technical field of spice finishing. Background technique [0002] Maoxiang Extract, Medicinal Rhinoceros Extract, Grain Raingrass Extract, Tonka Bean Tincture, etc. are all traditional flavoring materials for tobacco. They have been widely used in flavoring various tobacco products. These spices can inhibit the irritation of tobacco. , improve the taste of smoke, supplement the aroma of smoke, and its aroma-enhancing effect is very significant, and is deeply loved by perfumers. In recent years, the use of these flavors in the tobacco flavor industry has dropped significantly, and some have even been banned, because these flavors all contain a common ingredient-coumarin. [0003] Coumarin, also known as benzoα-pyrone, is a bicyclic compound synthesized from a benzene ring and an oxygen heterocycle. Coumarins are a class of aromatic compounds that widely ex...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/10
CPCC07D311/10
Inventor 赵世兴黄艳陈志雄林德洪郑作略胡武
Owner 澳华达香精(广州)有限公司
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