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Method for preparing phytostanol ester under solvent-free condition

A technology of phytostanol ester and phytostanol, which is applied in the fields of medicine, chemical industry, cosmetics and food, can solve the problems of harsh reaction conditions of catalysts, high corrosion of equipment, environmental pollution, etc., and achieves easy purification and esterification of products. High efficiency and simple process effect

Inactive Publication Date: 2013-05-29
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The use of the above catalysts has harsh reaction conditions (high temperature, long time), low yield, and great corrosion to equipment and serious environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 0.1202g of lauric acid, 0.2073g of phytostanols and 1.0mol% (relative to the molar weight of phytostanols) scandium trifluoromethanesulfonate in a 25mL reaction test tube with a branched port, and place with magnetic stirring In a constant temperature oil bath, the reaction was stirred at 120° C. for 4 h under nitrogen, and samples were taken every 0.5 h, and the reaction progress was detected by HPLC and TCL. After the reaction, a crude phytostanol ester product is obtained, which is separated and purified by column chromatography to obtain a phytostanol ester product, and its structure is identified by infrared, mass spectrometry and nuclear magnetic resonance spectrum analysis.

Embodiment 2

[0029] Add 0.1695g of oleic acid, 0.2073g phytostanols and 2.0mol% (relative to the molar weight of phytostanols) ferric trichloride in a 25mL reaction test tube with a branched port, place in a constant temperature oil with magnetic stirring In the bath, the reaction was stirred at 120° C. for 6 h under nitrogen, and samples were taken every 0.5 h, and the reaction progress was detected by HPLC and TCL. After the reaction, a crude phytostanol ester product is obtained, which is separated and purified by column chromatography to obtain a phytostanol ester product, and its structure is identified by infrared, mass spectrometry and nuclear magnetic resonance spectrum analysis.

Embodiment 3

[0031] Add 0.1883g of linoleic acid, 0.2073g phytostanols and 1.5mol% (relative to the molar weight of phytostanols) copper dodecyl sulfate in a 25mL reaction test tube with a branched port, place it under magnetic stirring In a constant temperature oil bath, stir the reaction at 130°C under nitrogen for 5 hours, take samples every 0.5 hours, use TCL to detect the reaction progress, use HPLC to measure the esterification rate and olefin by-product content, and measure the anisidine content of the reactant at the same time value to examine the degree of oxidation in the reaction system. After the reaction, a crude phytostanol ester product is obtained, which is separated and purified by column chromatography to obtain a phytostanol ester product, and its structure is identified by infrared, mass spectrometry and nuclear magnetic resonance spectrum analysis.

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Abstract

The invention relates to a method for preparing phytostanol ester under the solvent-free condition and belongs to the technical fields of food, medicine, chemical industry and cosmetics. According to the technical scheme, the method comprises the following steps of: adding fatty acid or aromatic acid, phytostanol and a catalyst at a certain molar ratio to a reaction tube with branched openings under the solvent-free condition; putting the reaction tube into a thermostatic oil bath with a magnetic stirring function; stirring for a certain time at a certain temperature in the atmosphere of nitrogen to enable materials to react to generate the product which is the phytostanol ester, wherein the phytostanol ester is generated after the reaction ends, the addition amount of the catalyst is 0.5-5.0mol% (relative to the molar weight of the phytostanol ester), the reaction temperature is 90-170 DEG C, and the reaction time lasts for 2-7 hours; sampling at fixed time, and measuring the conversion rate and the anisidine value to detect the reaction process; analyzing the product by infrared spectrum, mass spectrum and nuclear magnetic resonance spectrum to indentify the structure of the product, wherein the product is obtained by separating and purifying through column chromatography. The method is simple in process and high in efficiency and is suitable for large-scale production.

Description

technical field [0001] The invention relates to a green preparation method of phytostanol esters under solvent-free conditions, and belongs to the technical fields of food, medicine, chemical industry, cosmetics and the like. Background technique [0002] Phytosterols are a class of steroidal compounds with cyclopentaneperhydrophenanthrene as the main skeleton. Its structure is similar to cholesterol in animals. The US FDA has approved that foods added with phytosterols or stanol esters can use health labels. Adding it to special food as a functional food has the effect of lowering the concentration of total cholesterol and low-density lipoprotein cholesterol (LDL). Hydrogenated phytostanols are more hydrophobic than phytosterols and can more effectively increase cholesterol secretion and excretion. Plant stanols have low solubility and are hardly absorbed in the body, so they will not increase blood cholesterol, and stanols will not be transformed into substances similar t...

Claims

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Application Information

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IPC IPC(8): C07J75/00C07J9/00
Inventor 贾承胜周阳何文森张晓鸣冯骉
Owner JIANGNAN UNIV
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