改进HPLC法测定雷替曲塞原料药中的光学异构体

Determination of Optical Isomers in Raltitrexed Raw Material by Modified HPLC

目的:改进高效液相色谱法测定雷替曲塞原料药中的光学异构体。方法:对色谱柱、流动相和进样量进行改进,改进后的色谱柱为CHIRALPAK AD-H,流动相为正己烷-无水乙醇-三氟乙酸(70∶30∶0.1,V/V/V),进样量为100μL,流速为1.0 mL/min,检测波长为226 nm,柱温为35℃。结果:光学异构体检测进样量线性范围为99.68~398.7 ng(r=0.999 9);定量限为4.945 ng,检测限为1.648 ng;精密度、稳定性、重复性试验的RSD<1.0%;加样回收率为99.43%~100.14%(RSD=0.25%,n=9)。结论:改进后的方法简便、准确、灵敏度高、重复性好,可用于测定雷替曲塞原料药中的光学异构体。

OBJECTIVE：To improve HPLC method for determining optical isomers in raltitrexed raw material. METHODS：After improved,the column was CHIRALPAK AD-H with mobile phase consisted of n-hexane-anhydrous ethanol-trifluoroacetate（70∶30∶0.1,V/V/V）. The sample size was 100 μL. The flow rate of 1.0 mL/min. The detection wavelength was set at 226 nm,and column temperature was 35 ℃. RESULTS：The linear range of optical isomers was 99.68-398.7 ng（r=0.999 9）. The quantitation limit was 4.945 ng,and detection limit was 1.648 ng. RSDs of precision,stability and reproducibility tests were all lower than1.0%;the recoveries ranged 99.43%-100.14%（RSD=0.25%,n=9）. CONCLUSIONS：The optimized method is simple,accurate,sensitive and reproducible,which can be used for the determination of optical isomers in raltitrexed raw material.