顶空气相色谱法测定甲磺酸帕珠沙星中1,2-二溴乙烷

目的建立顶空气相色谱法测定甲磺酸帕珠沙星中1,2-二溴乙烷。方法采用聚乙二醇毛细管色谱柱(30 m×530μm×1.0μm);柱温80℃;进样口温度200℃;FID检测器,检测器温度250℃;顶空进样,平衡温度80℃,平衡时间40 min;以水为溶剂测定甲磺酸帕珠沙星原料药中1,2-二溴乙烷的残留量。结果在此色谱条件下,1,2-二溴乙烷在2~10μg/mL(r=0.9996)范围内线性良好;平均回收率97.0%。结论本法简便、快速、准确,可有效检测甲磺酸帕珠沙星中残留的1,2-二溴乙烷。

Determination of Ethylene Dibromide in Pazufloxacin Mesylate by Headspace Gas Chromatography

Objective To establish a headspace gas chromatography method for the determination of ethylene dibromide in pazufloxacin mesylate. Methods The residual solvents in pazufloxacin mesylate were separated on macrogol capillary column（30 m × 530 μm ×1.0 μm） with an FID detector. The column temperature was set at 80 ℃. The injector and detector temperature were set at 200 and 250 ℃, respectively. The containers of headspace injector were in equilibrium for 40 min at 80 ℃. The water without organics was used as solvent. Results Good linearity of ethylene dibromide was obtained within the range of 2-10 μg/mL（r=0.9996）. The average recovery was 97.0 %. Conclusion The established method is simple, rapid and accurate, which can be used for the determination of ethylene dibromide in pazufloxacin mesylate.