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氧基酸杂质的方法。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、0.25mol/LNaOH、1.0mol/LNaAc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3.1~67.1nmol/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。
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.
出处
《分析测试学报》
CAS
CSCD
北大核心
2007年第6期862-865,共4页
Journal of Instrumental Analysis
基金
黑龙江省教育厅科学技术研究项目(10551103)
关键词
离子交换色谱
安培检测
氨基酸
缬氨酸
anion-exchange chromatography
amperometric detection
amino acids
valine
作者简介
于泓(1963-),男,黑龙江哈尔滨人,教授,博士,Tel:0451—88060570,E - mail: yuhonghsd@ yahoo. com. cn