洛索洛芬钠杂质2-[(4-乙酰基苯基)甲基]环戊酮研究

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 μm),流动相为乙腈-水(45:55),流速20 mL·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 C₁₈ column (21.1 mm×250 mm,5μm) with a mobile phase of acetonitrile-water (45:55) at the flow rate of 20 mL·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.

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