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Method for preparing high-content d-gamma-tocopherol from mixed tocopherol concentrate

A technology of tocopherol and concentrated solution is applied in the field of preparation of high-content d-γ-tocopherol monomers, can solve the problems of unsuitability for industrialized production, difficult to scale up for industrialization, high equipment requirements and the like, and achieves simple steps, low consumption, Low raw material requirements

Active Publication Date: 2018-08-21
浙江可明生物医药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This type of method does not directly use mixed tocopherols as raw materials for separation, but a chemical reaction occurs, and the process is relatively complicated, so it is not easy to scale up industrially
[0009] As can be seen from the above, there are many patent documents about the high-purity mixed tocopherols and tocopherol homologue monomers obtained by separation and purification in natural VE at present. These methods each have their advantages, but there are also many defects. To a large number of organic solvents, some have high requirements on equipment, and some have low yields, which are not suitable for industrial production

Method used

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  • Method for preparing high-content d-gamma-tocopherol from mixed tocopherol concentrate
  • Method for preparing high-content d-gamma-tocopherol from mixed tocopherol concentrate
  • Method for preparing high-content d-gamma-tocopherol from mixed tocopherol concentrate

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Embodiment 1

[0035] ·Instrument: medium and low pressure preparative chromatography system (generally refers to pressure ≤ 2.0Mpa is medium and low pressure, Suzhou Lisui Technology Co., Ltd., EZ Purifier 100 / 200 medium pressure purification system), stainless steel column Fill 300.0g of "Chromatorex MB" series of non-bonded spherical silica gel produced by Fuji, with a column volume of 650ml (1BV), a particle size of 40-75μm, and a pore size of Add a small amount of cyclohexane, fill it into the chromatography column, and the column volume is regarded as 550ml (ie 1BV=550ml). Use 3 times the cyclohexane (1650ml) of chromatographic column volume to elute and compact the equilibrated chromatographic column, then 75.0g mixed tocopherol concentrate (total tocopherol content 50.5%, wherein γ-tocopherol relative content 63.8%) (The mixed tocopherol raw material comes from Xinchang Pharmaceutical Factory) and 75mL cyclohexane to dissolve and load the sample, continue to elute with 2BV cyclohex...

Embodiment 2

[0040] Instrument: medium and low pressure preparative chromatography system (Suzhou Lisui Technology Co., Ltd., EZ Purifier 100 / 200 medium pressure purification system), stainless steel column Filled with 300.0g SiliCycle "SiliaFlash" series of non-bonded spherical silica gel, column volume 650ml (1BV), particle size 40-75μm, pore size

[0041] The chromatographic column was equilibrated according to the method of Example 1. After the chromatographic column in Example 1 was equilibrated, 50.0 g of mixed tocopherol concentrate (total tocopherol content 70.5%, wherein the relative content of γ-tocopherol was 63.8%) was added to 100 ml of n-heptane, dissolved and loaded. After loading the sample, continue to elute with 1.5BV of n-heptane hexane, collect eluent I and eluent II in sections; 2BV 30% first-class tert-butyl ether and n-heptane mixed solution elution collected eluent II and eluent III; then eluted with 2BV first-class tert-butyl ether to obtain eluent IV, and fina...

Embodiment 3

[0044] Instrument: medium and low pressure preparative chromatography system (Suzhou Lisui Technology Co., Ltd., EZ Purifier 100 / 200 medium pressure purification system), stainless steel column Filled with 300.0g SiliCycle "SiliaFlash" series of non-bonded spherical silica gel, column volume 650ml (1BV), particle size 40-75μm, pore size

[0045] The chromatographic column was equilibrated according to the method of Example 1. After equilibrating the chromatographic column according to the steps in Example 1, add 30.0 g of mixed tocopherol concentrate (total tocopherol content 90.5%, wherein the relative content of γ-tocopherol is 70.0%) into 15 ml of n-hexane, dissolve and load the sample. After loading the sample, continue to elute with 1.5BV of n-hexane, and collect eluent I and eluent II in sections; The mixed solution is eluted to collect eluent II and eluent III; then eluted with 2BV of ether to obtain eluent IV, and finally equilibrated with 2BV of n-hexane, and the ...

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Abstract

The invention discloses a method for preparing high-content d-gamma-tocopherol from a mixed tocopherol concentrate. In conventional methods, a part of the methods use a great amount of organic solvents; a part of the methods have high requirements on equipment; and a part of the methods are low in yield and are not applicable to industrial production. According to the invention, the mixed tocopherol concentrate is dissolved in a low-polarity organic solvent, and then silica-gel preparative chromatography is carried out; then the low-polarity organic solvent is added to elute unadsorbed impurities; then eluants of different concentrations are used for gradient elution; and solvents are segmentally collected and recovered so as to obtain a monomer product with mixed tocopherol content of noless than 90% and gamma-tocopherol content of no less than 80%. According to the invention, the mixed tocopherol concentrate is used as a raw material and subjected to silica-gel column chromatographic separation once so as to obtain the high-content d-gamma-tocopherol. The method is simple in extraction process, and overcomes the problems of difficulties in recovery and indiscriminate applicationof solvents in traditional processes, great environmental pollution, low separation efficiency, etc.

Description

technical field [0001] The invention relates to a production method of natural VE, in particular to a preparation method of high-content d-γ-tocopherol monomer. Background technique [0002] Vitamin E (Vitamin E, referred to as VE), also known as anti-sterility vitamin, is a general term for tocopherol, tocotrienol and d-α-tocopherol active derivatives, widely present in animal and vegetable fats, organs, and vegetable oils In materials and chlorophyll plants. As the raw material for extracting natural VE, the deodorized distillate of vegetable oil (DD oil) is the main source of industrially extracted natural VE. Due to the complex components in DD oil and the minimal structural differences among the various homologues of natural VE, only mixed tocopherols can be obtained by traditional separation methods, and it is difficult to obtain high-purity natural VE and its various homologues monomer. The physiological activities, functions and antioxidant properties of each toco...

Claims

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Application Information

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IPC IPC(8): C07D311/72
CPCC07D311/72
Inventor 代志凯李祥清马金萍王义永许新德邵斌
Owner 浙江可明生物医药有限公司
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