洛索洛芬钠杂质2-[(4-乙酰基苯基)甲基]环戊酮研究

Study on the impurity 2-[(4-acetyl-phenyl) methyl]cyclopentanone of loxoprofen sodium

目的:对洛索洛芬钠的杂质2-[(4-乙酰基苯基)甲基]环戊酮进行研究。方法:洛索洛芬钠与醋酸水浴反应生成杂质,制备液相色谱采用Sepax Sapphire C18柱(21.1 mm×250 mm,5!m),流动相为乙腈-水(45∶55),流速20 m L·min-1,检测波长254 nm,柱温为室温。收集目标物后旋转蒸发并减压干燥,经紫外光谱、红外光谱、离子肼-飞行时间质谱与核磁共振谱对杂质进行结构确认。结果:通过实验确认该杂质结构为2-[(4-乙酰基苯基)甲基]环戊酮。结论:该杂质应予以控制。

Objective： To study 2-[（ 4-acetyl-phenyl） methyl] cyclopentanone,which is an impurity of loxoprofen sodium. Methods： The impurity was obtained through the reaction between loxoprofen sodium and acetic acid heated in boiling water bath. The preparative HPLC system consisted of a Sepax Sapphire C18column（ 21. 1 mm × 250 mm,5!m） with a mobile phase of acetonitrile-water（ 45∶ 55） at the flow rate of 20 m L·min-1. The detection wavelength was 254 nm and the column temperature was room temperature. The impurity was collected and dried by rotary evaporation. UV,IR,LC / MS-IT-TOF and NMR were used to confirm the structure of loxoprofen impurity. Results： The chemical structure of loxoprofen sodium impurity was confirmed to be 2-[（ 4-acetylphenyl） methyl]cyclopentanone.Conclusion： This impurity should be controlled in loxoprofen sodium.