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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: To establish a method for the analysis of ketoprofen enantiomers by precolumn derivatization reversed-phase high performance liquid chromatography. Methods: After derivatisation of S - (+) - ketoprofen and R - (-) ketoprofen with thionyl chloride and S - (-) - 1- A pair of diastereomers is generated. Hypersil C18 column was used, with acetonitrile-water-acetic acid-triethylamine (5 8:42:01:0 0 2) as the mobile phase and detected at 254nm. Chromatographic fractions were verified by electrospray ion trap mass spectrometry. Results: The retention times of the diastereomer peaks were 73 min and 85 min, respectively, and the resolution was 19. Conclusion: The derivatized product is stable, its sensitivity is high, reproducibility is good, and its operation is simple. It can be used for drug quality control and enantioselective pharmacokinetic study.