柱前衍生化高效液相色谱手性固定相法拆分手性氰醇

Enantioseparation of chiral cyanohydrin enantiomers on chiral stationary phase by precolumn derivatization-high performance liquid chromatography

利用正相高效液相色谱法在多糖衍生物手性固定相(OJ-H、OD-H、AD-H或AS-H)上成功地分离了一系列(31个)氰醇对映体的乙酰化或丙酰化衍生物,并拆分了3个脂肪族氰醇对映体的乙酰化衍生物。探讨了这些外消旋体在这四支手性柱上的色谱行为,通过考察流动相组成、流速、进样浓度和温度等因素对对映体拆分效果的影响,优化了色谱分离条件。方法已应用于脂肪酶催化转酯化拆分反应中手性氰醇衍生物的光学纯度的鉴定。

A series of enantiomer cyanohydrin esters were successfttlly separated by polysaccharide derivatives based chiral stationary phase （OJ-H, OD-H, AD-H or AS-H） under normal phase high performance liquid chromatographic （HPLC） conditions. The acetic anhydride and propionate anhydride were used as derivatives reagents. The chromato- graphic parameters of these racemates on OJ-H, OD-H, AD-H and AS-H columns were examined. Through investigation on the influence of the composition of the mobile phase, the flow rate, the injected concentration on the enanti- omer retentivity and selectivity and the column temperature on the chiral separation, the chromatographic conditions were optimized. This method has been applied to determining the optical purity of resolution of transesterification of chiral cyanohydrin by lipase.