亚苄基海因水解制备苯丙酮酸过程的色-质联用分析

针对亚苄基海因水解体系建立了一种高效实用的液相色谱分析方法,为生产工艺控制提供了依据,并应用液-质联用技术对此体系中的未知副产物进行了初步检测。具体液相色谱条件为:流动相:乙腈 -5mmol·L-1乙酸盐缓冲液(用醋酸调pH4 5 ),流速 0 5mL·L-1;梯度洗脱;色谱柱:AgilentEclipseXDB-C8, 5μm, 4 6×150mm, 20℃;二极管阵列检测器,检测波长: 204nm。色-质联用中质谱条件为:ESI离子源,负离子模式;气帘气流量1 03×105 Pa,电喷雾电压-4 200V,离子源温度 500℃,辅助雾化气 1 37×105 Pa,干燥气 4 13×105 Pa,相对分子质量检测范围:m/z40~600。液相色谱法测定亚苄基海因和苯丙酮酸的线性相关系数为0 999 05和0 999 86,亚苄基海因和苯丙酮酸的平均回收率为 101 45 %和 97 23 %,相对标准偏差为 1 002%和0 833 8%。精密度以相对标准偏差来表示,分别为0 591 9 % 和0 648 2 %。结果表明,该液相色谱分析方法简便、快速,结果准确,可以用于苯丙酮酸生产的质量控制。

Process analysis of preparation of phenylpyruvic acid by hydrolysis of 5-benzalhydantoin by LC-MS

The preparation of phenylpyruvic acid by hydrolysis of 5-benzalhydantoin was studied. A sensitive HPLC method has been developed for the quantitative determination of phenylpyruvic acid and 5-benzalhydantoin first, then based on the HPLC method, the whole hydrolysis system has been determined by HPLC-MS.The results showed that the linearity correlation coefficients of phenylpyruvic acid and 5-benzalhydantoin are (0.999 05) and (0.999 86). Average recover rate:101.45%,97.23%,RSD:1.002%,(0.833 8%). Precision RSD:(0.591 9%),(0.648 2%). So the HPLC method offered a sensitive and specific tool for the qualificaion of phenylpyruvic acid and 5-benzalhydantoin in industrial production.