磷酸三乙胺-乙腈流动相体系反相分离2，4-二硝基氟苯-氨基酸衍生物

Reversed-phase Separation of 2,4-dinitrofluorobenzene-amino Acid Derivatives with Triethylamine Phosphate/ACN Mobile Phase

中文关键词:  液相色谱  柱前衍生  反相分离  氨基酸  2，4-二硝基氟苯

英文关键词:liquid chromatography  pre-column derivatization  reversed-phase separation  amino acids  2,4-dinitrofluorobenzene

中文摘要:

      从两个方面改进了反相分离2，4-二硝基氟苯-氨基酸衍生物测定氨基酸的分析方法：一是使用高缓冲容量pH 2.75和6.50的磷酸三乙胺-乙腈流动相体系代替醋酸盐/乙腈流动相体系；另一个是强调了衍生反应的操作细节。以含精、丝、天冬、谷、苏、甘、丙、脯、组、蛋、缬、色、苯丙、亮、异亮、赖、酪氨酸注射液为目标试样，对方法进行认证，线性不低于0.9999(对谷氨酸、赖氨酸和酪氨酸不低于0.9998)，准确度（回收率）为100±1%，精密度（RSD）低于0.5%，均优于以往的方法。方法适用于在一般液相色谱实验室进行氨基酸注射液和原料药的分析，无需专用氨基酸分析仪。

英文摘要:

      In this work, the analytical method for the determination of amino acids by the reversed-phase separation of 2,4-dinitrofluorobenzene-amino acid derivatives has been improved in two aspects: one is the use of triethylamine phosphate(pH 2.75 and 6.50)/ACN mobile phase with high buffer capacity instead of the acetate/ACN system, another is the operation details of derivatization is stressed. The new developed method is superior to the previous one in linearity, accuracy and precision. With an injection containing Arg, Ser, Asp, Glu, Thr, Gly, Ala, Pro, His, Met, Val, Trp, Phe, Leu, Ile, Lys and Tyr as the target sample, the method has been validated to show that its linearity, accuracy and precision are ≧0.9999(≧0.9998 for Glu, Lys and Tyr), 100±1% and ≦0.5%, respectively. Without the requirement of special AA analyzer, the method is applicable to the analysis of amino acid injections and bulk drugs in the general LC laboratory.