N-（N-苯甲酰基-O-苯甲酰基-L-酪氨酰基）-L-苯丙氨醇及其异构体的手性高效液相色谱分析

建立了正相高效液相色谱法（NP-HPLC）测定中间体N-（N-苯甲酰基-O-苯甲酰基-L-酪氨酰基）-L-苯丙氨醇（M057）及其三个异构体M1、M2、M3含量的方法.采用CHIRALPAK（R）IA手性柱,正己烷-异丙醇（75∶25）为流动相,流速0.5 mL/min,检测波长231 nm.M057在浓度0.106～1.063 μg/mL范围内与峰面积呈良好的线性关系（r=0.9999）,平均回收率100.31％,RSD为1.66％;检出限5.67 ng/mL.异构体M1、M2、M3检出限分别为10.00、9.67、10.00 ng/mL.本法准确、简便、重现性好,适用于该中间体光学纯度的检测.

Determination of N-（N-benzoyl-O-benzoyl-L-tyrosyl）-L-phenylalaninol and Its Stereoisomers by Chiral High Performance Liquid Chromatography

A normal phase high performance liquid chromatography （NP-HPLC）method for the determination of N-（N-benzoyl-O-benzoyI-L- tyrosyl）-L-phenylalaninol （M057） and its stereoisomers M l, M2 and M3 was developed. Separation was achieved on a CFtlRALPAKC 1A column using a n-hexane ： isopropyl alcohol （75 ： 25, w/v） mobile phase with the flow rate of 0.5 ink/rain. The UV detector wavelength was set at 231 rim. The standard curve was prepared with six calibrators over a concentration range of 0.106-1.063 ~g/mL for M057. Regression equation revealed linear relationship （correlation coefficient： 0.99991 between the peak area of the analyte and the concentration. The average recovery was 100.31% with RSD 1.66 % for M057. The limits of detection were 5.67 ng/mk for M057, 10.00 ng/mL fnr MI, 9.67 ng/mL for M2 and 10.00 ng/mL for M3. The method was accurate, simple and repeatability, and was suitable for the optical purity control of the intermediate.