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 than 1.0%; 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.
关键词
雷替曲塞原料药光学异构体高效液相色谱法方法改进
Keywords
Raltitrexed raw materialOptical isomersHPLCMethod improvement