Separation and purification method for mixed tocopherols

A purification method and technology for tocopherol, which are applied in the field of separation engineering, can solve the problems of complicated purification process, high cost, unsatisfactory separation effect of separation monomer purity, etc., and achieve the effects of cost reduction, simple steps and good quality.

Active Publication Date: 2015-04-22
NINGBO DAHONGYING BIO ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a mixed tocopherol product with simple operation, low cost, high purity of the separated monomer and good overall yield, aiming at the problems of complicated and high cost of the current purification process, separation effect and unsatisfactory purity of the separated monomer. Separation and purification method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 50g of mixed tocopherols containing 50% of natural vitamin E to a mixed solvent of 200g of methanol and ethyl acetate to form a column solution with a mass concentration of 10%, wherein the mass percentage of methanol and ethyl acetate is 9:1 .

[0033] After the obtained upper column liquid is applied to the column, the flow rate is controlled at 30-35 drops / minute to ensure that the residence time of the upper column liquid in the resin column is 3 hours.

[0034] Elute with a mixed solvent of 500g ethanol and n-hexane, wherein the mass percentage of ethanol and n-hexane is 19:1, collect and obtain 302.1g eluent I; then use 300g ethanol solution containing 5% acetic acid by mass percentage for elution , and collected 311.5g of eluent II; the obtained eluent I and eluent II were distilled off the solvent under reduced pressure to obtain 15.2g of d-(β+γ) tocopherol monomer respectively, and the total content of natural vitamin E was 90.2 %, its relative content is ...

Embodiment 2

[0036] Add 50 g of mixed tocopherols containing 30% of natural vitamin E to a mixed solvent of 300 g of ethanol and n-hexane to prepare a column solution with a mass concentration of 7.14%, wherein the mass percentage of ethanol and n-hexane is 19:1.

[0037] After the obtained upper column liquid is applied to the column, the flow rate is controlled at 45-50 drops / minute to ensure that the residence time of the upper column liquid in the resin column is 2 hours.

[0038] Elute with a mixed solvent of 500g of isopropanol and n-hexane, wherein the mass percentage of isopropanol and n-hexane is 9:1, collect and obtain 397.6g of eluent I; then use 300g of ethanol solution containing 4% by mass of propionic acid After elution, 306.2g of eluent II was collected; the obtained eluent I and eluent II were evaporated to remove the solvent under reduced pressure, and 9.5g of d-(β+γ) tocopherol monomer, natural vitamin E total The content is 86.4%, its relative content is 86.9%, and d-de...

Embodiment 3

[0040] Add 50g of mixed tocopherols containing 40% of natural vitamin E to 200g of methanol and n-hexane mixed solvent to prepare a column solution with a mass concentration of 8%, wherein the mass percentage of methanol and n-hexane is 19:1.

[0041] After the obtained upper column liquid is applied to the column, the flow rate is controlled at 8-10 drops / minute to ensure that the residence time of the upper column liquid in the resin column is 10 hours.

[0042]Eluted with a mixed solvent of 600g ethanol and n-hexane, wherein the mass percentage of ethanol and n-hexane was 4:1, and 395.2g eluent I was collected; then eluted with 300g methanol solution containing 6% acetic acid by mass percentage , and collected 310.5g of eluent II; the obtained eluent I and eluent II were evaporated to remove the solvent under reduced pressure, respectively, to obtain 13.7g of d-(β+γ) tocopherol monomer, and the total content of natural vitamin E was 85.9 %, its relative content is 86.3%, an...

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Abstract

The invention discloses a separation and purification method for mixed tocopherols. The method adopts an anion exchange resin column for purification and includes the following steps: dissolving the mixed tocopherols in a solvent A; preparing a sample solution with the mass percent of 5%-20% for sampling; using a solvent B to elute the anion exchange resin column after the sample solution remains in the resin column for 1-10h, and obtaining an elution I through collection; using a solvent C to elute the anion exchange resin column, and obtaining an elution II through collection; and decompressing the elution I and the elution II to steam the solvents and obtain d-(beta+gamma) tocopherols and d-delta tocopherols. The method is adopted for separation and purification, the extraction process is simple, the cost is low, the environmental pollution is small, the purity of the d-(beta+gamma) tocopherols monomer and the d-delta tocopherols monomer obtained through the extraction is high, and the total yield of the mixed tocopherols is high.

Description

technical field [0001] The invention relates to the technical field of separation engineering, in particular to a separation and purification method of mixed tocopherols. Background technique [0002] Vitamin E, also known as tocopherol, is one of the essential vitamins for the human body. It includes 8 kinds of substances such as α, β, δ, and γ-type tocopherols and corresponding tocotrienols. It has the functions of scavenging free radicals, anti-cancer and anti-cardiovascular disease, boost immunity and anti-aging effects. There are two types of sources of vitamin E: chemical synthesis and natural products. Natural vitamin E is a dextrorotary form with physiological activity, that is, d-form, while the synthetic product is a racemic form, that is, a mixture of d-form and l-form. The biological activity of natural vitamin E is more than twice that of synthetic products, and bioabsorption The degree is also higher than synthetic products, and has better food safety. [00...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C07D311/72
Inventor张源仁王燕峰王嘉磊
OwnerNINGBO DAHONGYING BIO ENG