新型含苯并噻唑α-氨基膦酸酯类化合物在淀粉类手性固定相上的液相色谱分离

本文运用涂敷型(Chiralpak AD-H)和键合型(Chiralpak IA)两种淀粉类手性固定相高效液相色谱法，进行了新型含苯并噻唑α-氨基膦酸酯类化合物的手性分离。从色谱分离的保留因子(k)、分离系数(α)和分离度(Rs)三个方面考察了两种类型色谱柱的分离性能，上述化合物在Chiralpak IA柱上能够得到较好的基线分离。同时，讨论了温度、流动相极性和目标分析物的结构等因素对Chiralpak IA柱分离性能的影响。由于键合型固定相较稳定的性能，使某些非常规的溶剂(如THF)成功地应用于手性α-氨基膦酸酯类化合物的分离。

Chiral Separation of Novel α ‐Aminophosphonates Containing a Benzothiazole Moiety by Liquid Chromatography Using an Amylose Stationary Phase

The present report describes a chiral HPLC method for the enantiomeric separation of α‐aminophosphonate derivatives using two new coated and immobilized amylose‐based chiral stationary phases (CSP, Chiralpak IA and Chiralpak AD‐H). The chromatographic parameters such as retention factor (k), separation factor (α), and resolution (R_s) of the solutes were investigated on these two CSPs. Reasonably good baseline separation for these compounds was achieved using Chiralpak IA column. The influences of temperature, content of ethanol modifier and the structure of analyte were also studied. THF, EtOAc and CH₂Cl₂ were used as eluents on analytical and semi‐preparative columns. Highly enriched enantiomers with purities of up to 96.4% –100% (ee) and yields of 90.2% –95.5% were obtained, respectively. The proposed methods were found to be suitable and accurate for rapid separation and semi‐preparation of enantiomeric α‐aminophosphonate derivatives available.