Column chromatography isolation method for VA acetate, perhydride VA acetate and isomers thereof

A technology of acetate and column chromatography, applied in the direction of organic chemistry, can solve the problems of low VA acetate content and yield, inability to further direct crystallization, high energy consumption of process recovery, etc. much effect

Inactive Publication Date: 2018-06-29
SHANGYU NHU BIOCHEM IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] When VA acetate is prepared in the existing mature technology, the product VA acetate crude oil will be obtained. After an appropriate amount of absolute ethanol is dissolved and crystallized at low temperature, the by-product VA acetate mother liquor can be obtained, and the content of VA acetate is 30-50 %, but there are still perhydroVA acetate and its isomers and other impurities in the mother liquor, which cannot be further directly crystallized. In the past, because it could not be purified and utilized, the crystallization mother liquor was directly discarded, resulting in a waste of resources
[0005] The method provided by U.S. patent document US2676903A adopts acetonitrile-petroleum ether extraction system, but acetonitrile has high toxicity, high price, high energy consumption for process recovery, and the content and yield of VA acetate obtained are relatively low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0025] Preparation of the original mother liquor of VA acetate

[0026] Add 100g of VA acetate crude oil into a four-necked flask, add 150ml of absolute ethanol solvent, stir at a speed of 500r / min for 10min, then adjust the stirring speed to 80r / min, put the four-necked flask into a low-temperature thermostat to cool down, and the temperature drops to At -30°C, keep warm for another 12 hours, then take out the four-necked flask, filter and crystallize with suction to obtain a by-product VA acetate mother liquor solution, recover the dry solvent to obtain 38.9 g of VA acetate mother liquor.

Embodiment 1

[0028] Put 250g of silica gel into 400ml of n-hexane, stir for 2min, and then put it into a chromatography column (column height 50cm, inner diameter 4cm). Adjust the n-hexane liquid level in the chromatography column to just cover the top of the silica gel.

[0029] Mother liquor pretreatment: dissolving 20 g of the original mother liquor of VA acetate in 20 ml of n-hexane solvent, the mass content of VA acetate is 45%, the mass content of perhydroVA acetate and its isomers is 32%, and the mass content of other impurities is 23%.

[0030] Column chromatography separation: Add the above pretreated mother liquor to a silica gel chromatography column, elute with 18% methanol-82% n-hexane (v / v), control the flow rate at 5-10ml / min, and the eluent passes through the liquid phase Chromatography and ultraviolet spectrophotometer qualitative analysis, collected 355ml of high-content VA eluent, and the eluent was concentrated and recovered by rotary evaporator to obtain 12.05g of high...

Embodiment 2

[0033] Put 250g of silica gel into 400ml of n-hexane, stir for 2min, and then put it into a chromatography column (column height 50cm, inner diameter 4cm). Adjust the n-hexane liquid level in the chromatography column to just cover the top of the silica gel.

[0034] Mother liquor pretreatment: dissolving 20g of the original mother liquor of VA acetate in 20ml of n-hexane solvent, the mass content of VA acetate is 45%, the mass content of perhydroVA acetate and its isomers is 32%, and the mass content of other impurities is 23%;

[0035] Column chromatography separation: Add the above-mentioned pretreated mother liquor to a silica gel chromatography column, elute with 2% methanol-98% n-hexane (v / v), control the flow rate at 5-10ml / min, and the eluent passes through the liquid phase Chromatography and ultraviolet spectrophotometer qualitative analysis, collected 360ml of high-content VA eluent, and the eluent was concentrated and recovered by rotary evaporator to obtain 11.23g ...

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Abstract

The invention relates to a column chromatography isolation method for VA acetate, perhydride VA acetate and isomers thereof. The method comprises the following steps: (1) dissolving a VA acetate mother solution into a non-polar solvent in the volume ratio of (1 to 2):1 to obtain a pretreated mother solution; (2) adding the pretreated mother solution in the step (1) onto a silica gel chromatographycolumn, using an eluent to carry out elution, controlling the flow rate to be 5 to 10 mol / min, carrying out qualitative analysis on the eluant by using a liquid chromatogram and ultraviolet spectrophotometer, and collecting high-content VA elutant, wherein the elutant is a mixed liquor of at least one non-polar solvent and at least one polar solvent; (3) carrying out concentration recycling on the VA elutant obtained in the step (2) so as to obtain a high-content refined VA acetate mother solution. The content of the high-content refined VA acetate mother solution obtained by the method can reach 80% or higher, and the yield can reach 90% or higher.

Description

technical field [0001] The invention relates to a separation process of vitamin A acetate, in particular to a method for separating VA acetate, perhydroVA acetate and its isomers by column chromatography. Background technique [0002] Vitamin A Acetate (Vitamin A Acetate), also known as vitamin A acetate or retinol acetate, is a kind of light yellow fine spherical particle powder with good fluidity, no peculiar smell, easy to oxidize in the air, and exposed to light Perishable. [0003] VA acetate is used for vitamin A deficiency. It is an essential factor to regulate the growth and health of epithelial tissue cells. It can maintain the normal metabolism of the human body, maintain the stability and development of cell membranes, and maintain the normal function of the reproductive system. It can be used for skin care, wrinkle removal, Whitening and other advanced cosmetics. At the same time, vitamin A acetate can increase the health of vision, ensure the good comfort of t...

Claims

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Application Information

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IPC IPC(8): C07C403/12
CPCC07C403/12
Inventor 王成龙吕国锋黄国东管敏虾罗江桥章萍萍
Owner SHANGYU NHU BIOCHEM IND
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