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A method for continuous chromatographic separation of tocopherol monomers

A continuous chromatography and tocopherol technology, applied in separation methods, chemical instruments and methods, solid adsorbent liquid separation, etc., to achieve stable performance, meet the requirements of large-scale continuous production, and high feasibility of industrial scale-up

Active Publication Date: 2019-12-31
COFCO GROUP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the defect in the prior art that continuous chromatography cannot be used to obtain different types of tocopherol monomers at one time, and to provide a method for continuous chromatography to separate tocopherol monomers, wherein the continuous chromatography includes A feed area and an elution area comprising a plurality of elution units, the method comprises: injecting the raw material liquid of the crude mixed tocopherol product from the inlet of the feed area into the continuous chromatogram, and passing through the elution solvent in the plurality of elution units respectively. Each elution unit is eluted, and each elution unit is only eluted for one tocopherol monomer

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  • A method for continuous chromatographic separation of tocopherol monomers
  • A method for continuous chromatographic separation of tocopherol monomers
  • A method for continuous chromatographic separation of tocopherol monomers

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preparation example Construction

[0023] In the present invention, the method for preparing the raw material liquid of the crude mixed tocopherol product may include: mixing the crude mixed tocopherol product with solvent I.

[0024] In the present invention, the ratio of the crude mixed tocopherol product to the solvent I is not particularly limited, and can be a conventional choice in the art. For example, relative to 1 kg of mixed tocopherols, the amount of solvent I can be 0.5-10 L, preferably 0.8-5 L.

[0025] In the present invention, the type of the solvent I can be a conventional choice in the art, for example, the solvent I can be methanol, ethanol, n-propanol, isopropanol, propenol, acetone, hexane, ethyl acetate and one or more of petroleum ether, preferably one or more of methanol, ethanol, ethyl acetate and acetone.

[0026] In the present invention, the definition of the crude product of mixed tocopherols can be conventionally understood in the field. For example, the mixed tocopherols may be n...

Embodiment approach

[0036] According to a specific embodiment, the mixed tocopherols contain two tocopherol monomers, α-tocopherol and β / γ-tocopherol, and α-tocopherol is separated in the first elution unit, and the Deunitization separates β / γ-tocopherol. The elution solvent includes elution solvent I used in the first elution unit and elution solvent II used in the second elution unit. The elution solvent I can be at least one of methanol, ethanol, isopropanol, n-propanol, propenol and acetonitrile, and the elution solvent II can be formed by the elution solvent I and acid according to the ratio of 100ml:0-10g The mixture, preferably 100ml: 0-1g, more preferably 100ml: 0.01-1g. Preferably, the elution solvent I is different from the washing solvent and solvent I. The number of chromatographic columns in the first elution unit and the second elution unit is not particularly limited, and may be one or more columns each. In order to achieve a better separation effect, preferably, the first eluti...

Embodiment 1

[0070] This example is used to illustrate the method for continuous chromatographic separation of tocopherol monomers provided by the present invention

[0071] This embodiment adopts figure 2 The rotary disc type continuous chromatographic separation device of shown 10 post 6 districts (operating area), described continuous chromatogram comprises feeding area (1 chromatographic column), washing impurity area (1 chromatographic column), the first elution unit ( 1 chromatographic column), the second elution unit (3 chromatographic columns, connected in series), the 3rd elution unit (1 chromatographic column) and the regeneration area, the regeneration area includes the acid removal unit (1 chromatographic column), alkali regeneration unit (1 column) and alkali removal unit (1 column). Type I macroporous strong base anion exchange resin is used as the separation medium; the mixed tocopherol crude product used is the mixed tocopherol obtained from vegetable oil deodorization di...

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Abstract

The invention relates to the field of tocopherol and discloses a method for separating tocopherol monomers with a continuous chromatograph. The continuous chromatograph comprises a feeding area and aneluting area, and multiple eluting units are contained in the eluting area. The method comprises steps as follows: a raw material solution mixed with a crude tocopherol product is injected into the continuous chromatograph through an inlet of the feeding area and is eluted in the multiple eluting units respectively by an elution solvent, and each eluting unit is only used for eluting one kind oftocopherol monomer. With adoption of the technical scheme, alpha-tocopherol, beta / gamma-tocopherol and delta-tocopherol with high purity and high recovery rate can be obtained through continuous separation based on the continuous chromatograph, product quality is stable, solvent consumption is low, resin utilization rate is high, and the products are applicable to industrialized enlargement.

Description

technical field [0001] The invention relates to the field of tocopherols, in particular to a method for continuous chromatographic separation of tocopherol monomers. Background technique [0002] Tocopherol is an essential fat-soluble vitamin that belongs to the vitamin E family. Its chemical structure is: a 6-hydroxyl chromanol (6-hydroxyl chroman) and a saturated C substituted at the 2' position of the chroman ring 16 side chain. According to the position and number of methyl groups on the chromanol benzene ring, tocopherol can be divided into α-, β-, γ- and δ-tocopherol. Naturally occurring tocopherol is generally a mixture of 3-4 monomers. β-tocopherol and γ-tocopherol are species-dependent, and generally do not exist in the same crop or oil at the same time. [0003] Tocopherol has strong antioxidant properties, can improve animal fertility, and has significant effects in preventing cancer, preventing and treating cardiovascular and cerebrovascular diseases, and anti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D311/72B01D15/10
CPCB01D15/10C07D311/72
Inventor 车夏宁丁子元许克家林海龙曹玉平陈学兵周学晋刘安妮
Owner COFCO GROUP
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