Refining method of novel menthol

A refining method and menthol technology, applied in directions such as being fixed on/in an organic carrier, fermentation, etc., can solve the problems of free enzyme survival temperature, narrow pH value range, easy inactivation and denaturation, insufficient stability and the like, To achieve the effect of good smoke effect, high optical purity and mild process conditions

Inactive Publication Date: 2017-03-22
HUBEI CHINA TOBACCO IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Free enzymes survive in a narrow range of temperature and pH, are not stable enough to heat, strong acid, strong alkali, organic solvents, etc., are easily inactivated and denatured, and there are other insurmountable shortcomings in the catalytic reaction. For modern industry Say free enzyme is not an ideal catalyst

Method used

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  • Refining method of novel menthol
  • Refining method of novel menthol
  • Refining method of novel menthol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Take ethyl acetate and menthol with a molar ratio of 1:1, dissolve it in absolute ethanol with 4.5 times the total mass of ethyl acetate and menthol, heat and reflux for 10 hours, and spin off the solvent after stopping the reaction Ethanol, obtains thick product, elutes 3 times with distilled water, obtains menthyl ester;

[0028] (2) Take sodium alginate, add 50 times its weight in distilled water, oscillate to dissolve, then add 1.2% of its weight in sodium periodate, and react in the dark at 4°C for 24 hours to obtain oxidized sodium alginate, and the obtained oxidized The degree of oxidation of sodium alginate is 0.9%;

[0029] (3) Drop the oxidized sodium alginate into 2% calcium chloride solution of 10 times its mass, soak for 35 minutes, wash with distilled water 3 times and dialyze, and filter to obtain calcium alginate microspheres;

[0030] (4) Take 10 mg of lipase, add / 0.1 g calcium alginate microspheres obtained in step (3), dissolve in a buffer soluti...

Embodiment 2

[0033](1) Take ethyl acetate and menthol with a molar ratio of 1.4:1, dissolve it in dehydrated ethanol with 4.5 times the total mass of ethyl acetate and menthol, heat and reflux for 10 hours, stop the reaction and spin off the solvent Ethanol, obtains thick product, elutes 3 times with distilled water, obtains menthyl ester;

[0034] (2) Take sodium alginate, add 50 times its weight in distilled water, oscillate to dissolve, then add 5.4% of its weight in sodium periodate, and react in the dark at 4°C for 24 hours to obtain oxidized sodium alginate, and the obtained oxidized The degree of oxidation of sodium alginate is 4.7%;

[0035] (3) Drop the oxidized sodium alginate into 3% calcium chloride solution of 20 times its mass, soak for 50 min, wash with distilled water 3 times and dialyze, and filter to obtain calcium alginate microspheres;

[0036] (4) Take 16 mg of lipase, add 0.1 g of the calcium alginate microspheres obtained in step (3), dissolve in a buffer solution o...

Embodiment 3

[0039] (1) Take ethyl acetate and menthol with a molar ratio of 2:1, dissolve it in absolute ethanol with 4.5 times the total mass of ethyl acetate and menthol, heat and reflux for 10 hours, and spin off the solvent after stopping the reaction Ethanol, obtains thick product, elutes 3 times with distilled water, obtains menthyl ester;

[0040] (2) Take sodium alginate, add 50 times its weight of distilled water, shake and dissolve, then add 10% of its weight of sodium periodate, and react in the dark at 4°C for 24 hours to obtain oxidized sodium alginate, and the obtained oxidized The degree of oxidation of sodium alginate is 9.5%;

[0041] (3) Drop oxidized sodium alginate into 4% calcium chloride solution of 50 times its mass, soak for 55 minutes, wash with distilled water 3 times and dialyze, and filter to obtain calcium alginate microspheres;

[0042] (4) Get 26mg of lipase, add 0.1g of calcium alginate microspheres obtained in step (3), dissolve in a buffer solution of pH...

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Abstract

The invention provides a refining method of novel menthol. The refining method comprises the following steps: (1) carrying out esterification reaction on menthol, thus synthesizing menthyl acrylate; (2) synthesizing a modified calcium alginate gel carrier, and fixing lipase through the calcium alginate gel carrier; and (3) carrying out chiral resolution on menthol by adopting the fixed lipase, thus obtaining L-menthol. According to the refining method provided by the invention, the used raw materials are safe, the resolution selectivity is high, and the prepared L-menthol is high in optical purity and good in effect when used for cigarettes; the technological conditions are mild, the product can be recycled for a plurality of times, and the application prospect is wide.

Description

technical field [0001] The invention belongs to the field of spice preparation, in particular to a novel method for refining menthol. Background technique [0002] Organisms perceive the aroma of spices and essences through enzymes in the organism or receptor molecules on the cell surface, and the enzymes in the organism or receptor molecules on the cell surface are chiral molecules, and their basic units are carbohydrates Compounds, amino acids, etc. are also chiral, so compounds with the same chemical structure have different aromas due to their different chiralities. In 1961, Ohloff published the aroma properties of the first chiral fragrance (+)-β-citronellol 1. (+)-1 has citronellal fragrance, (-)-1 has geranium oil fragrance. Subsequently, it was discovered that the different enantiomers could exhibit different fragrances or different degrees of fragrance. Chiral fragrances with different optical purity can also exhibit different odor thresholds. The importance of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P41/00C12P7/22C12N11/10
Inventor 王娜司辉董爱君谢豪周湘熊国玺张耀华
Owner HUBEI CHINA TOBACCO IND
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