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Preparation method of vitamin B5 crude product

A vitamin and crude product technology, which is applied in the field of preparation of vitamin B5 crude product, can solve the problems of affecting the extraction yield, poor effect, and easy emulsification reaction, etc., and achieves strong operability, increased crystallization yield, and reduced environmental pollution. Effect

Active Publication Date: 2018-01-26
NINGXIA KINGVIT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the above enzymatic hydrolysis splitting process of DL-pantoate lactone, it is generally necessary to extract and separate D-pantoate and L-pantoate lactone. During the extraction process, emulsification reactions are prone to occur: when slightly emulsified , you need to add an appropriate amount of activated carbon, sodium chloride saturated brine, etc., and stand for a long time to achieve effective separation; when the emulsification is severe, the effect is not good
In addition, adding activated carbon is easy to adsorb D-pantoic acid, which affects the extraction yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Take 300ml of DL-pantolactone enzymatic hydrolysis solution (containing 6.6% (g / ml) of D-pantoic acid), and feed the DL-pantotolactone enzymatic hydrolysis solution into the macroporous adsorption resin at a feed rate of 2BV / h, L-pantoic acid lactone is adsorbed on the column and separated from D-pantoic acid, and top washed with 30% (g / g) methanol until no D-pantoic acid flows out, and D-pantoic acid is obtained 360ml of 5.4% (g / ml) solution is used for the following experiments. The L-pantolactone adsorbed by the macroporous adsorption resin is analyzed with petroleum ether-pentyl propionate composite solvent (volume ratio 3:1), the analysis speed is 0.5BV / h, the analysis solution is collected, and the solvent is recovered by concentration under reduced pressure to obtain L-pantolactone, processed separately. The yield of D-pantoic acid was 98.2%.

[0035] The D-pantothenic acid solution obtained by separating the above macroporous adsorption resin is filtered thro...

Embodiment 2

[0039] Take 300ml of DL-pantolactone enzymatic hydrolysis (containing 6.6% (g / ml) of D-pantoic acid), and feed the DL-pantolactone enzymatic hydrolysis into the macroporous adsorption resin at a feed rate of 3BV / h, top wash with 30% (g / g) methanol until no D-pantoic acid flows out, and obtain 355ml of a 5.5% (g / ml) solution containing D-pantoic acid, which is used for the following experiments. The L-pantolactone adsorbed by the macroporous adsorption resin was analyzed with petroleum ether-pentyl propionate composite solvent (volume ratio 3:1), the analysis speed was 1.0BV / h, the analysis solution was collected, and the solvent was recovered by concentration under reduced pressure to obtain L-pantolactone, processed separately. The yield of D-pantoic acid was 98.5%.

[0040] The 5.5% (g / ml) D-pantothenic acid solution obtained by separating the above macroporous adsorption resin is filtered through a plate frame (filter cloth pre-laid with 2.5cm thick perlite), a carbon col...

Embodiment 3

[0044] Take 300ml of DL-pantolactone enzymatic hydrolysis solution (containing 6.6% (g / ml) of D-pantoic acid), and feed the DL-pantotolactone enzymatic hydrolysis solution into the macroporous adsorption resin at a feed rate of 4BV / h, top wash with 30% (g / g) methanol until no D-pantoic acid is detected to flow out, and 352ml of 5.4% (g / ml) D-pantoic acid solution is obtained. for the following experiments. The L-pantolactone adsorbed by the macroporous adsorption resin was analyzed with petroleum ether-amyl propionate composite solvent (volume ratio 3:1), the analysis speed was 1.5BV / h, the analysis solution was collected, and the solvent was recovered by concentration under reduced pressure to obtain L-pantolactone, processed separately. The yield of D-pantoic acid was 96.5%.

[0045] The 5.4% (g / ml) D-pantothenic acid solution obtained by separating the above macroporous adsorption resin is passed through a plate frame (filter cloth pre-laid with 3cm thick perlite), a car...

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Abstract

The invention relates to a preparation method of a vitamin B5 crude product. The preparation method comprises the process steps of carrying out adsorption separation on DL-pantolactone enzymatic hydrolysate by virtue of macroporous adsorption resin, and carrying out purification, filtration, lactonization, solvent extraction, D-calcium pantothenate synthesis and vacuum drying, so as to obtain theVB5 crude product. The method for separating and extracting D-pantoic acid and L-pantolactone by virtue of the macroporous adsorption resin has beneficial effects that the problems that the quality and yield are reduced due to the emulsion easily occurring in an extraction process are overcome; meanwhile, VB5 is separated out by virtue of a solvent-method crystallization technique, so that the crystallization time is shortened, the extraction yield is increased, the product quality is improved, and the economic benefit is increased; and the method is simple and convenient, low in solvent loss,strong in operability and suitable for industrial production, and the environmental pollution can be reduced.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, in particular to a vitamin B 5 Method for the preparation of the crude product. Background technique [0002] Vitamin B 5 (VB5), also known as D-calcium pantothenate, chemical name D-N-(2,4-dihydroxy-3,3-dimethylbutyryl)-β-alanine calcium), relative molecular weight: 476.54. Calcium pantothenate can be divided into three types: DL-type (mixed body), D-type (dextral body), and L-type (left-handed body), of which only the D-type (dextral body) has biological activity. [0003] VB5 is an odorless, slightly bitter white powder. Its specific rotation +25 0 ~+28 0 ; Melting point 159~160℃; Soluble in water and glycerin, slightly soluble in ethanol, chloroform and ether; Unstable under acidic and alkaline conditions, very stable under neutral (pH5.0~7.0) conditions; Thermal stability. [0004] VB5 enters the human body to release calcium and pantothenic acid, and pantothenic acid is the precurso...

Claims

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Application Information

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IPC IPC(8): C07C231/02C07C235/12
Inventor 裴立忠王智王锋徐强周志伟
Owner NINGXIA KINGVIT PHARMA
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