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Preparation method of phytosterol in ionic liquid

A technology of phytosterol ester and ionic liquid, which is applied in the preparation of steroids, chemical instruments and methods, steroids, etc., can solve the problems of high price, and achieve the effects of simple operation, high yield and mild reaction conditions

Inactive Publication Date: 2012-07-25
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Common ionic liquids include imidazole-type ionic liquids, such as [Bmim]BF 4 ,[Bmim] CF 3 SO 3 , but more expensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 1.440g (7.2mmol) lauric acid, 0.984g (2.4mmol) phytosterol and 0.069g ChCl 2SnCl to the reaction flask with branch tube 2 (7% relative to the mass of phytosterols), placed in a constant temperature oil bath with magnetic stirring, stirred and reacted at 150° C. for 4 h under nitrogen, sampling every 0.5 h, and using HPLC and TCL to detect the reaction process. After the reaction, the crude phytosterol ester was obtained with a yield of 92.3%. The phytosterol ester product was obtained by separation and purification by column chromatography, and its structure was identified by infrared, mass spectrometry and nuclear magnetic resonance spectrum analysis.

Embodiment 2

[0027] Add 1.344g (4.8mmol) linoleic acid, 0.984g (2.4mmol) phytosterol and 0.079g ChCl 2.5SnCl to the reaction flask with branch tube 2 (8% relative to the mass of phytosterols), placed in a constant temperature oil bath with magnetic stirring, stirred and reacted at 160° C. for 4 h under nitrogen, sampling every 0.5 h, and using HPLC and TCL to detect the reaction process. After the reaction, the crude phytosterol ester was obtained with a yield of 90.5%. The phytosterol ester product was obtained by separation and purification by column chromatography, and its structure was identified by infrared, mass spectrometry and nuclear magnetic resonance spectrum analysis.

Embodiment 3

[0029] Add 0.864 (6.0 mmol) octanoic acid, 0.984 g (2.4 mmol) phytosterol and 0.059 g ChCl 2ZnCl to the reaction flask with branch tube 2 (6% relative to the mass of phytosterols), placed in a constant temperature oil bath with magnetic stirring, stirred and reacted at 120° C. for 4 h under nitrogen, sampling every 0.5 h, and using HPLC and TCL to detect the reaction process. After the reaction, the crude phytosterol ester was obtained with a yield of 88.6%. The phytosterol ester product was obtained by separation and purification by column chromatography, and its structure was identified by infrared, mass spectrometry and nuclear magnetic resonance spectrum analysis.

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Abstract

The invention relates to a preparation method of phytosterol in ionic liquid, belonging to the technical field of food, medicines, chemical industries, cosmetics and the like. The preparation method adopts the following technical scheme: a certain amount of fatty acid, phytosterol and ionic liquid are added in a reaction bottle which is provided with a magnetic stirrer and a branch tube, nitrogen is introduced, the mixture in the reaction bottle is heated to certain temperature, then the timing is started, and the reaction stops after being conducted for a while. The dosage of the ionic liquid is 5-10% of the weight of the phytosterol, the reaction temperature is 90 DEG C-170 DEG C, and the reaction time is 2-8h. The sampling is conducted at regular time, and the reaction process is detected by TLC (The-Layer Chromatography) qualitative analysis and HPLC (High-Performance Liquid Chromatography) quantitative analysis. After the reaction is finished, an upper phase and a lower phase are formed in a reaction bottle, a reactant and a reaction product are arranged in the upper layer and are subjected to chromatographic separation and purification to obtain the phytosterol, and the structure of the phytosterol is identified through the analysis of infrared ray, mass spectrum and nuclear magnetic resonance spectrum; and the lower layer is the ionic liquid which can be recycled. According to the preparation method, the environmental protection is achieved, the yield is high, the operation is simple, and the scale production is convenient.

Description

technical field [0001] The invention relates to a green preparation method of phytosterol esters in ionic liquids, and belongs to the technical fields of food, medicine, chemical industry, cosmetics and the like. Background technique [0002] Because of their similar structure to cholesterol, phytosterols can competitively inhibit the absorption of cholesterol in the small intestine, thereby effectively reducing the absorption of total blood cholesterol and low-density lipoprotein cholesterol. As a dietary therapy, phytosterols can be taken at the beginning of cholesterol-lowering treatment. However, free phytosterols have a high melting point and poor fat-solubility and water-solubility, which limits its practical application range. The C-3 hydroxyl group of sterol is an important active group, which can form fatty sterol ester with fatty acid. Studies have shown that fatty acid phytosterol esters are more fat-soluble and can also inhibit the absorption of cholesterol. ...

Claims

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Application Information

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IPC IPC(8): C07J9/00C07J75/00
Inventor 贾承胜刘萍郭素洁周阳
Owner JIANGNAN UNIV
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