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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。
Benzoyl chloride was used as a derivatization reagent to derivatize phenylalanine as an amide enantiomer. Quinine was used as a chiral ion pair reagent and ion-pair chromatography was performed on a silica gel column to successfully separate DL-β-benzene Alanine enantiomers. At the same time, qualitative analysis was carried out using the law of chromatographic retention and spectral characteristic absorption curves. The effects of mobile phase composition on the retention and separation selectivity were investigated. The experimental results showed that the concentration of quinine had little effect on the retention and separation selectivity in the range of 0.19-0.73 mmol / L. However, A smaller increase in concentration can result in a decrease in retention and separation selectivity; an increase in acetic acid concentration also results in a decrease in retention and separation selectivity. The mobile phase consisted of dichloromethane with n-pentanol ratio of 99/1, containing 0.35 mmol / L of quinine, the proportion of acetic acid in the mobile phase was 3/100 and the flow rate was 1.8 mL / min The phenylalanine derivative has an enantiomeric resolution of 1.30 and a selectivity of 1.18.