Preparation of high content mixed tocopherols

Abstract

The invention discloses a method for extracting mixed tocopherols with high content form raw materials with low content of tocopherols. In the existing methods, the amount of some used solvents is too large, some methods have excessive requirements on equipment and some methods are too small in yield, thus being inapplicable to industrialized production. In the invention, deodorizing distillate of fatty acid oil is subjected to esterification and alcoholysis firstly and then freezing and crystallization are carried out to separate out phytosterol; then, after aliphatic ester in a filtrate is reclaimed by short-path distillation, a tocopherol concentrate is obtained and separated by silica gel column chromatography, and eluted with three organic solvents of different polarity so as to obtain the aliphatic ester, the mixed tocopherols with high content and phytosterol crude product. The method of the invention has low requirements on raw materials, is easy for large-scale industrialized production, and can obtain high content of mixed tocopherols and obtain fatty acid methyl ester and phytosterol.

Description

technical field [0001] The invention relates to the preparation of tocopherols, in particular to an industrialized method for extracting high-content mixed tocopherols from raw materials with low tocopherol content. Background technique [0002] Natural vitamin E (Vitamin E) is the most important fat-soluble vitamin, it can only be synthesized in plants, it is a very important dietary supplement for humans and animals, and sometimes it is also used as a medicine. Natural vitamin E can be divided into tocopherols and tocotrienols according to the presence or absence of double bonds on their side bond groups. Tocopherols generally exist in common vegetable oils (such as soybean oil, sunflower oil, corn germ oil and rapeseed oil). oil, etc.), while tocotrienols are higher in cereal seeds (such as oats, barley, rye, and rice bran), and are highest in palm oil. Both tocopherol and tocotrienol are a mixture containing four active isomers of α, β, γ, and δ. Since the content of n...

AI Technical Summary

Problems solved by technology

In this method, the operation steps are relatively cumbersome, a variety of organic solvents are used, and the requirements for raw materials are high, and the effect of fixed bed esterification is not very good.

[0006] The method disclosed in CN1,234,703C is to remove free fatty acids through multiple esterification reactions, then remove sterols through twice freezing and crystallization after saponification, and finally obtain mixed tocopherols by adsorption method. This method has many steps, a large amount of solvent, and The yield of the product obtained is low

[0007] US3,122,565, US5,487,817 and US3,402,182 all use strongly basic anion exchange resins to increase the content of mixed tocopherols, but an obvious shortcoming of using anion exchange resins is exactly: a large amount of organic solvents will be used, there is an acid In the process of elution and alkali regeneration, the loading capacity of the resin is low and the service life is short, which limits its industrial application

[0008] US4,550,183 and EP0,171,009 consider refining mixed tocopherols by solvent extraction, which will use a large amount of organic solvents, which will inevitably bring certain environmental pollution, and the yield of the product is not high