顶空气相色谱法测定注射用甲磺酸吉米沙星中基因毒性杂质

Determination of Genotoxic Impurities in Gemil oxacin Mesylate for Injection by Head-space GC

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 head-space GC method for the determination of the genotoxie impurities in gernifloxacin mesylate for injection.Methods： A Supelco capillary column （30 m×250 μm, 0.25 μm） （temperature programming）, nitrogen as carrier gas （flow rate： 0.5 mL.min-1） and uECD（temperature： 250 ℃ ） were used. H-space sampling was conducted （equilibrium temperature： 60 ℃, equilibrium time： 30 min, injection port temperature： 1 10 ℃, injection volume： 1 mL ） with a split ratio of 1：10. Results： The genotoxic impurities, methyl methanesulfonate, ethyl methanesulfonate and isopropyl methanesulfonate showed good linear relationships m the limitationn range of 20%-120%.Their LOQs were 0.010 0, 0.250 0 and 1.250 0μg.L-1 respectively. Their LODs were 0.002 0, 0.010 0, 0.250 0 μg,L-1 respectively. Their average recoveries were 99.20%, 99.45% and 99.98%（n=9）. Conclusion： The method is accurate and convenient. It is suitable for the determination and limitation control of the genotoxic impurities in gemifloxacin mesylate.