摘要
以苯甲酰氯为衍生试剂，将苯丙氨酸衍生为酰胺对映体，用奎宁作为手性离子对试剂，应用离子对色谱法，在硅胶柱上，成功地分离了DL-β-苯丙氨酸对映体，同时利用色谱保留值规律和光谱特征吸收曲线综合进行了定性分析。考察了流动相组成对保留值和分离选择性的影响，实验结果表明，在0.19～0．73mmol/L范围内，奎宁浓度对保留值和分离选择性影响不大；而流动相中戊醇浓度之较小增加即可导致保留值与分离选择性下降；醋酸浓度增加亦导致保留值与分离选择性降低。选用流动相组成：二氯甲烷与正戊醇的比例为99/1，内含0．35mmol/L的奎宁，醋酸在流动相中的比例为3／100，流量为1．8mＬ/min时，苯丙氨酸衍生物对映体分离度为1．30，分离选择性为1．18。
The ion-pair chromatographic separation of the enantiomer of DL-β-phenylalanine has been studied by deriving amidefrom Phenglalanine, using benzoyl chloride as derivative agent, in the ZORBAX SIL column and using quinine as chiral ion-pair agent. The qualitative analysis has been done with the chromatographic retention value rule and the spectrographic absorption curves by photodiode array detector. The experimental results showed that the concentration of quinine from 0.19 to 0. 73 mmol/l had little effect on the retention and separation selectivity, the small increase of the concentration of 1-pentanol and acetic acid in the mobile phase led to the decreaes of retention and separation selectivity.The ratio between dichloromethane and 1-pentanol in the elected mobile phase is 99/1, containing qUinine (0. 35 mmol/L) and acetic acid (3/100), The separation degree of the derivative of DL-β-Phenylalanine was 1. 30 in the flow rate 1. 8 mL/min and separetion selectivity was 1.18.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2000年第2期133-136,共4页
Chinese Journal of Analytical Chemistry
