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目的:建立测定注射用甲磺酸吉米沙星中甲磺酸烷基酯类基因毒性杂质的顶空气相色谱法。方法:以Supelco毛细管柱(30m×250μm,0.25μm)为色谱柱,程序升温;氮气为载气,流速为0.5mL·min-1;采用微池电子捕获检测器,检测器温度为250℃;顶空进样,平衡温度为60℃,平衡时间为30min,进样口温度为110℃,进样量为1mL;分流比为1:10。结果:基因毒性杂质甲磺酸甲酯、甲磺酸乙酯和甲磺酸异丙酯在限度为20%~120%的范围内线性关系良好,定量限分别为0.0100、0.2500和1.2500μg·L-1,检测限分别为0.0020、0.0100和0.2500μg·L-1,平均回收率分别为99.20%、99.45%和99.98%(n=9)。结论:该方法准确、简便,适用于甲磺酸吉米沙星中基因毒性杂质的检测及限度控制。
OBJECTIVE: To establish a headspace gas chromatographic method for the determination of genotoxicity of alkyl mesylate in gemifloxacin mesylate for injection. METHODS: Supelco capillary column (30 μm × 250 μm, 0.25 μm) was used as the chromatographic column and the temperature was programmed. Nitrogen gas was used as the carrier gas and the flow rate was 0.5 μL · min-1. Micro-cell electron capture detector The temperature of the sample was 250 ° C. The headspace sample was taken. The equilibrium temperature was 60 ° C, the equilibration time was 30 min, the inlet temperature was 110 ° C, and the injection volume was 1 μL. The split ratio was 1:10. Results: The genotoxic impurities methyl methanesulfonate, ethyl methanesulfonate and isopropyl methanesulfonate showed good linearity in the range of 20% -120% with the limits of quantitation of 0.010-0.0, 0.250-0 And the average recoveries were 99.20%, 99.45% and 99.98%, respectively (n = 9) and 1.250? 0 μg · L-1 with the detection limits of 0.002,0.0,0.0,0,0 and 0.250,0 μg? L-1, respectively ). Conclusion: The method is accurate and simple and is suitable for the detection and limit control of genotoxic impurities in gemifloxacin mesylate.