Method for preparing lyral for cosmetic testing

A technology of lyral and crude products, which is applied in the detection of cosmetics, especially the detection of allergenic fragrances in cosmetics, can solve the problems of inconvenient use, expensive reference substances, and difficulty in obtaining them

Active Publication Date: 2021-11-09
江西省药品检验检测研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the one hand, this reference substance is expensive and difficult to obtain, for example, it usually needs to be purchased from abroad; on the other hand, since lyral is a volatile oil, it is inconvenient to use as a reference substance, for example, it is very inconvenient in precision sampling , I

Method used

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  • Method for preparing lyral for cosmetic testing
  • Method for preparing lyral for cosmetic testing
  • Method for preparing lyral for cosmetic testing

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0095] Add 539g (3.5mol) myrcenol and 0.539g hydroquinone in the 1000mL four-necked flask that thermometer, mechanical stirring device and reflux condenser are equipped with, be heated to 110 ℃; In described myrcenol, dropwise add 235g ( 4.2 mol) of acrolein was added dropwise for 6 hours. During the dropwise addition, the reaction bottle was placed in a freezing tank, and the temperature of the reaction bottle was kept at 110°C to 130°C; after the dropwise addition of acrolein was completed, the reaction was continued for 1 hour to obtain mixture;

[0096] The reaction mixture was washed three times with 200g deionized water to obtain 766g lyral crude product (GC recorded lyral content 94.32%); the crude product was rectified below vacuum tightness 2mmHg, and collected at 120° C. The fraction between 125° C. obtained 611 g of lyral (the content of lyral was 99.64% as measured by GC).

[0097] The obtained lyral fraction (about 1 / 4 amount, multiplied by the remainder for late...

Embodiment 2

[0099]Add 539g (3.5mol) myrcenyl alcohol and 0.539g hydroquinone in the 1000mL four-necked flask that thermometer, mechanical stirring device and reflux condenser are equipped with, be heated to 110 ℃; In described myrcenyl alcohol, dropwise add 216g ( 3.86 mol) of acrolein, added dropwise for 6 hours. During the dropwise addition, the reaction bottle was placed in a freezing tank, and the temperature of the reaction bottle was kept at 110°C to 130°C; after the dropwise addition of acrolein was completed, the reaction was continued for 1 hour to obtain mixture;

[0100] The reaction mixture was washed three times with 180g deionized water to obtain 757g lyral crude product (94.73% lyral content was recorded by GC); The fraction between 125° C. obtained 607 g of lyral (the content of lyral was 99.73% as measured by GC).

[0101] The obtained lyral fraction (about 1 / 4 amount, multiplied by the remainder for later use) is introduced into the sodium chloride powder that can pass ...

Embodiment 3

[0103] Add 539g (3.5mol) myrcenol and 0.539g hydroquinone in the 1000mL four-necked flask that thermometer, mechanical stirring device and reflux condenser are equipped with, be heated to 110 ℃; In described myrcenol, dropwise add 196g ( 3.5 mol) of acrolein was added dropwise for 6 hours. During the dropwise addition, the reaction bottle was placed in a freezing tank, and the temperature of the reaction bottle was kept at 110°C to 130°C; after the addition of acrolein was completed, the reaction was continued for 1 hour to obtain the reaction mixture;

[0104] The reaction mixture is washed three times with 180g deionized water to obtain 748g lyral crude product (GC records 88.76% lyral content); The fraction between 125° C. obtained 503 g of lyral (the content of lyral was 99.46% as measured by GC).

[0105] The obtained lyral fraction (about 1 / 4 amount, multiplied by the remainder for later use) is imported into the sodium chloride powder that can pass through a 200 mesh s...

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Abstract

The invention relates to a method for preparing lyral for cosmetic testing. The method comprises the following steps: (a) reacting myrcenyl alcohol with acrolein; (b) washing the reaction mixture with deionized water to obtain crude lyral; (c) rectifying the crude lyral to collect Lilial fractions between 120°C and 125°C to obtain refined lyral; (d) finely granulating the lyral fractions to obtain the final product. The product of the invention exhibits excellent physical and chemical characteristics, and has excellent stability, especially excellent volatilization stability.

Description

technical field [0001] The invention belongs to the technical field of cosmetics, and relates to a detection method for cosmetics, in particular to a detection method for detecting allergenic fragrances in cosmetics, especially cosmetics, and a method for preparing such fragrances. The prepared fragrances can be It is conveniently applied to the detection of this kind of fragrance in cosmetics or as an additive of some products. In particular, the allergenic fragrance is lyral. Background technique [0002] According to statistics, at least 35% of cosmetic allergies are allergies caused by fragrances. In response to the problems that may be caused by the use of spices, major relevant international agencies and organizations have issued corresponding regulations and policies to restrain the spices and flavors market. Flavors and fragrances are directly or indirectly related to "human health" and become the objects of compulsory management by governments of various countries...

Claims

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Application Information

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IPC IPC(8): C07C47/46C07C45/69C07C45/82G01N30/02G01N30/06
CPCC07C45/69C07C45/82C07C2601/16G01N30/02G01N30/06G01N2030/045C07C47/46
Inventor 易路遥章红晏亮程一鑫杨婷婷刘剑李杰虞雪军刘绪平潘蕾钟振华熊雯吉伟佳占翌领
Owner 江西省药品检验检测研究院
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