草酸水解聚唾液酸分离提纯制备N-乙酰神经氨酸

Separation and purification to prepare N-acetylneuraminic acid after oxalic acid hydrolysis of polysialic acid

为了探究草酸水解聚唾液酸分离提纯制备高纯度N-乙酰神经氨酸的工艺条件,以期简化工艺步骤和降低生产成本;作者重点考察了草酸对聚唾液酸的水解,首先对比了草酸和其他常规水解酸的水解效果,确定了草酸为聚唾液酸的水解酸.然后通过正交实验确定最佳草酸水解操作参数:水解温度为90℃、水解时间为3.5 h、水解酸浓度为0.1 mol/L和聚唾液酸稀释倍数为5倍,在此条件下,聚唾液酸的水解率平均可达94%以上,水解收率可达97%以上.通过实验条件及步骤优化,得到分离提纯制备高纯度N-乙酰神经氨酸的最佳工艺.在该工艺下,红外光谱及HPLC分析证实所得产品中主要成分是N-乙酰神经氨酸,其纯度为98.5%,收率为58.4%.

The polysialic acid was obtained from fermentation of escherichia coli,and hydrolyzed to separate,purify and prepare the N-acetylneuraminic acid.In order to study the process conditions of separation and purification to prepare high purity of n-acetylneuraminic acid from the polysialic acid which was hydrolyzed by the oxalic acid,so as to simplify the process and reduce the production cost,the authors investigated emphatically the hydrolysis of the polysialic acid by oxalic acid,contrasted firstly the effects on hydrolysis of polysialic acids between oxalic acids as other conventional hydrolytic acids and determined oxalic acids as hydrolytic acids.The best operating parameters of the oxalic acid hydrolysis of the polysialic acid was determined by the orthogonal experiment:hydrolysis temperature 90℃,hydrolysis time 3.5 h,hydrolysis acid concentration 0.1 mol/L and diluted multiples of polysialic acid 5 times.In these conditions,the hydrolyze rate of the polysialic acid was more than 94%,and the hydrolyze yield was more than 97%.The separation and purification conditions were optimized through experiments,and the separation and purification process for the preparation of high purity N-acetylneuraminic acid was obtained.In these process conditions,the analytic results of the infrared spectrum and HPLC showed that the purity of the N-acetylneuraminic acid product was 98.5%,and the yield was 58.4%.