【摘要】 在优化实验条件下,建立了高效阴离子交换色谱-积分脉冲安培检测法分离测定缬氨酸产品中微量氨基酸杂质的方法。研究了氨基酸的阴离子交换色谱分离和积分脉冲安培检测。采用优化的水、0.25 mol/LNaOH、1.0 mol/L NaAc三元梯度淋洗条件及35℃柱温实现了19种氨基酸的分离。在最佳条件下,氨基酸的检出限(S/N=3)为3.1~67.1 nmol/L,线性范围约为3个数量级。样品加标回收率为90%~96%。方法可以推广至其它氨基酸产品中微量氨基酸杂质的测定。更多还原

【Abstract】 A direct,sensitive,simple and practical method for determination of trace amino acid impurities in valine product by high-performance anion-exchange chromatography with integrated pulsed amperometric detection has been developed.The anion-exchange separation and integrated pulsed amperometric detection of amino acids were investigated.In order to separate amino acids,a ternary gradient with water,0.25 mol/L sodium hydroxide and 1.0 mol/L sodium acetate was employed.The optimized gradient eluent condition and column temperature(35 ℃) for analysis of 19 amino acids were obtained.Under optimized condition,detection limits(S/N=3) for 19 amino acids were 3.1-67.1 nmol/L.The calibration graphs of peak area for all the analytes were linear about three orders of magnitude.The recoveries of added standard were 90%-96%.The method is also used to determine trace amino acid impurities in other amino acid product.更多还原