Method for preparing high-purity natural vitamin E monomers by separating mixed tocopherol

Abstract

The invention discloses a method for preparing high-purity natural vitamin E monomers by separating mixed tocopherol. The method comprises the following steps of: fully dissolving the mixed tocopherol in a mobile phase solvent I so as to obtain a loading solution; adding the loading solution into a reversed-phase chromatographic column; adding a mobile phase solvent II into the chromatographic column; and performing step-by-step collection to obtain effluent I of which the purity of d-alpha-tocopherol is more than or equal to 90 percent, effluent II of which the purity of d-gamma-tocopherol is more than or equal to 90 percent and effluent III of which the purity of d-delta-tocopherol is more than or equal to 85 percent. By the method, the one-time column loading and separation of raw materials can be realized under normal pressure so as to obtain three natural vitamin E monomers. A filler in the chromatographic column can be regenerated, the used solvents can be recovered, the cost is reduced, the method is convenient to operate, and the purity is high.

Description

technical field [0001] The invention relates to a method for separating and preparing high-purity natural vitamin E monomer from mixed tocopherols. Background technique [0002] Natural vitamin E, also known as tocopherol, is a mixed tocopherol that mainly contains 8 isomers, namely α, β, γ, and δ tocopherols and α, β, γ, and δ tocotrienols. Natural vitamin E mainly exists in natural vegetable oils, and current research has found that the deodorized distillates of oils (DD oil for short) are rich in natural vitamin E. Due to the complex components in the deodorized effluent and the minimal structural differences among the various isomers of vitamin E, mixed tocopherols are often obtained by using general methods, and it is difficult to obtain various single forms of high-purity natural vitamin E. In order to obtain high-purity vitamin E monomers, the raw materials must be processed first, so that the target products can be concentrated into various vitamin E monomers as muc...

AI Technical Summary

Problems solved by technology

Because this method is not easy to control the switching time of valves in each interval, there are certain difficulties in the selection and recovery of solvents, especially the high cost of this equipment, and there is no report on the industrial separation of vitamin E in China.

[0004] CN101323067A discloses a method of using the deodorized distillate as a raw material, through esterification alcoholysis, cooling and crystallization to separate phytosterols, and recovering by short-path distillation, to prepare a tocopherol concentrate, and then to perform silica gel chromatography on the tocopherol concentrate Column separation, and then washing with different organic solvents to obtain fatty acid esters, high-content mixed tocopherols and phytosterols, but this method only obtains mixed tocopherols, and cannot obtain various monomers of tocopherols

[0005] CN1234703C discloses a method of taking deodorized distillate as raw material through hydrolysis acidification, methanol esterification, saponification, esterification, cooling, and finally separating fatty acid methyl ester through distillation, and then preparing mixed tocopherols by adsorption and separation, although this The purity of the tocopherol obtained by the method is more than 95%, but it is only a mixture of various tocopherol monomers, and various tocopherol monomers with higher purity cannot be obtained.