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Extraction method of tocopherol intermediate

A technology of tocopherol and intermediates, which is applied in the field of efficient extraction of tocopherol intermediates, can solve problems such as removal, achieve stable reaction process, stabilize production technology, and avoid oxidative deterioration

Inactive Publication Date: 2012-08-15
JIANGNAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Since the content of impurities such as glyceride and sterol ester in the tocopherol concentrate is too high, and its boiling point is similar to that of tocopherol, it cannot be removed by distillation and other operations

Method used

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  • Extraction method of tocopherol intermediate
  • Extraction method of tocopherol intermediate
  • Extraction method of tocopherol intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] All instruments and equipment are laboratory-scale. D-α-tocopherol accounts for 7.67% in the amine methylation product of tocopherol concentrated liquid, D-β, γ-tocopherol intermediates account for 61.06%, and D-δ-tocopherol intermediates body accounted for 26.97%.

[0038] Take 20g of tocopherol concentrated liquid amine-methylated product (about 30mL) into the reactor, add 50mL of aqueous solution with 90% acetic acid content, then add 60mL of n-heptane reagent, control the temperature at about 30°C, and stir for 0.5h; Then stand for stratification, the lower layer is the water phase of acetic acid, which is transferred to the desolventizer, heated to 120°C and distilled under reduced pressure to evaporate the acetic acid to obtain the non-D-α-tocopherol intermediate salt; finally add 10.7mL of mass The dimethylamine aqueous solution with a fraction of 40% was stirred at 35°C for 20 minutes, then the stirring was stopped, and 50 mL of deionized water was added to wash...

Embodiment 2

[0041]Take 20g of tocopherol concentrated liquid amine-methylated product (about 30mL) into the reactor, add 50mL of aqueous solution with 80% acetic acid content, then add 60mL of petroleum ether (60-90°C) reagent, control the temperature at about 35°C, Stir and react for 1.0 h; then stand to separate and separate, the lower layer is the aqueous phase of acetic acid, transfer it to the desolventizer, heat up to 120°C and distill the acetic acid under reduced pressure to obtain the non-D-α-tocopherol intermediate salt; Finally, add 10.7mL of dimethylamine aqueous solution with a mass fraction of 40%, stir at 35°C for 20min, stop stirring, add 50mL of deionized water to wash the feed solution and let it stand for stratification. The upper oil phase is the obtained non-α-tocopherol intermediate .

[0042] Take 1-2 drops of the product and weigh it and prepare 25mL diluted solution with absolute ethanol. Through reverse-phase high-performance liquid chromatography HPLC, using met...

Embodiment 3

[0044] Take 20g of tocopherol concentrated liquid amine-methylated product (about 30mL) into the reactor, add 60mL of aqueous solution with 80% propionic acid content, then add 60mL of n-hexane reagent, control the temperature at about 30°C, and stir for 1.0h; Then stand for stratification, the lower layer is the water phase of propionic acid, which is transferred to the desolventizer, heated up to 140 °C and distilled under reduced pressure to evaporate the propionic acid to obtain the non-D-α-tocopherol intermediate salt; finally add 10.7 40% aqueous solution of dimethylamine in mL was stirred at 35°C for 20 minutes, then the stirring was stopped, 50 mL of deionized water was added to wash the feed solution, and the mixture was allowed to stand for stratification. The upper oil phase was the obtained non-α-tocopherol intermediate.

[0045] Take 1-2 drops of the product and weigh it and prepare 25mL diluted solution with absolute ethanol. Through reverse-phase high-performance...

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Abstract

The invention relates to an extraction method of a tocopherol intermediate, belonging to the technical field of organic complexing extraction. The tocopherol intermediate is a product obtained after aminomethylation reaction of non-D-alpha-tocopherol in a tocopherol concentrated solution. The tocopherol concentrated solution contains higher-content mixed tocopherol (D-alpha, beta, gamma and delta-tocopherol), also contains a great amount of glyceride, fatty acid methyl ester, sterol ester and other impurities, and the preparation of high-content D-alpha-tocopherol is hindered by the existence of the impurities. The boiling points of the impurities are close to that of tocopherol, therefore, the impurities cannot be separated from tocopherol by distilling and other methods. The non-D-alpha-tocopherol intermediate is a tertiary amine substance, has certain alkalinity, and can be combined with an acid to form a salt, and glyceride and other impurities are easy to dissolve in an organic solvent. According to the invention, the tocopherol intermediate is extracted from glyceride and other impurities by a liquid-liquid extraction method, and the obtained non-D-alpha-tocopherol intermediate is almost pure, thus the purpose of purification is achieved.

Description

technical field [0001] The invention relates to a high-efficiency extraction method of a tocopherol intermediate. The extraction method achieves the purpose of efficiently separating a target product, and belongs to the technical field of organic complex extraction. Background technique [0002] Vitamin E, also known as tocopherol, has two types: synthetic and natural. Natural vitamin E is a mixture of four tocopherols and four tocopherol trienols, which is optically active; chemical synthetic products usually refer to DL-α-tocopherol, which is a racemic form of various optical isomers. body. Because natural vitamin E is superior to chemical synthetic products in terms of biological activity and safety, people tend to use natural vitamin E in medicine, food, cosmetics and feed additives. Therefore the present invention focuses on the development and utilization of research natural vitamin E. [0003] Tocopherol concentrate is a product purified from deodorized vegetable o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/72
Inventor 蒋平平李海洋董玉明印建国
Owner JIANGNAN UNIV
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