柱前衍生化-反相高效液相色谱法拆分酮洛芬对映异构体

Enantiospecific Analysis of Ketoprofen by RP-HPLC with Chiral Precolumn Derivatization

目的 :建立一种用柱前衍生化反相高效液相色谱法分析酮洛芬对映异构体的方法。方法 :采用二氯亚砜和S - (- )- 1- (1-萘基 )乙胺作为衍生化试剂 ,S - (+ ) -酮洛芬和R - (- )酮洛芬衍生化后生成一对非对映异构体。选用HypersilC18柱 ,以乙腈 -水 -乙酸 -三乙胺 (5 8∶42∶0 1∶0 0 2 )为流动相 ,在 2 5 4nm下检测。色谱流份经电喷雾离子阱多级质谱分析验证。结果 :非对映异构体色谱峰的保留时间分别为 7 3min和 8 5min ,分离度为 1 9。结论 :衍生化产物稳定 ,方法灵敏度高 ,重现性好 ,操作简单 ,可用于药品质量控制和对映体选择性药物动力学研究。

Objective:A RP-HPLC method has been developed for the determination of the R -and S -enantiomers of ketoprofen.Methods:The derivatization with thionyl chloride and S -(-)-1-(1-naphthyl)-ethylamine was followed by reversed-phase chromatography with a mobile phase of acetonitrile-water-acetic\|acid-triethylamine(55∶45∶0 1∶0 02 by vol)at a flow rate of 1 0 mL·min -1 and UV detection was performed at 254 nm.The electrospray ionization-quadrupole ion trap mass spectrometer was applied to verify the structure of derivatives of ketoprofen.Results:The retention times for the R -and S -ketoprofen diastereomeric amides were 7 3 and 8 5 min respectively with a resolution factor of 1 9 Conclusion:The present study provides a simple,reproducible and sensitive method for the quality evaluation of S -ketoprofen and enantiospecific pharmacokinetic studies.