高效液相色谱手性固定相的研究 Ⅰ.L-缬氨酸-叔丁酰胺型固定相的制备及对映体拆分

本文报道一种新型手性L-缬氨酸-叔丁酰胺型固定相的制备及用它直接拆分对映体的实验。实验结果表明,这种手性固定相对外消旋氨基酸衍生物有较好的拆分效果。洗脱液中异丙醇的含量对拆分效果有较大影响,异丙醇的含量增加,拆分效果下降。拆分样品的结构对总分离度(R_s)也有一定影响,在四种不同洗脱液系统中,DL-苯丙氨酸衍生物的R_s都比DL-缬氨酸衍生物和DL-亮氨酸衍生物小。流量0.6～2.0mL/min时对总分离度无明显影响。实验结果也证明,四种氨基酸衍生物都是D型的先洗脱。     

高效液相色谱手性固定相的研究 I:L-缬氨酸-叔丁酰胺型固定相的制备及对映体拆分

A new chiral chemically bonded stationary phase for direct resolution of optical isomers in HPLC was prepared. The experiemental data showed that the chiral stationary phase gave good resolution for the racemic α-amino acid derivatives and that there was no significant influence on the resolution as the eluting rate varied from 0.6 to 2.0 mL/min. The content of isopropanol in the eluent significantly affected the resolution of the enantiomers. The eluent consisting of 1% isopropanol in hexane gave most favorable result, but the retention times were a little longer. It is evident that the resolution was also influenced by the structure of the solute. In all cases, the resolution of N-Ac-DL-Phe-OMe is lower than that of N-Ac-DL-Leu-OMe and N-Ac-DL-Val-OMe. Although the capacity factor of N-Ac-DL-Tyr-Ome varied greatly in different eluting systems, the separation factor and resolution were very close. It was observed that D-amino acid derivatives eluted faster than the corresponding L-isomers. In the above chromatographic conditions N-acetyl-DL-α-phenylethylamine could not be resolved.