顶空气相色谱法测定甲磺酸加雷沙星中的甲磺酸乙酯残留

Determination of residues of ethyl methanesulfonate in garenoxacin mesylate by headspace gas chromatography

目的：建立甲磺酸加雷沙星中甲磺酸乙酯的气相色谱检测方法。方法：色谱系统采用AT-1000（30 m×0.53mm,1μm）气相色谱柱,ECD检测器,分流比为20∶1。结果：甲磺酸乙酯在37.56~338.04 ng/ml范围内线性关系良好（r=0.999 4）,平均回收率为99.5%,最低检测浓度为2.5 ng/ml。结论：该方法简便、准确、重现性好且专属性强。

Objective： To establish a gas chromatography（ GC） method for determining residues of ethyl methanesulfonate in garenoxacin mesylate. Methods： Ethyl methanesulfonate was quantitatively determined on a AT- 1000 column was（ 30 m × 0. 53 mm,1 μm） with column temperature being increased by programmed control; ECD was used as the detector with a split flow ratio of 20∶ 1. Results： The calibration curve was linear over the range of 37. 56 ~ 338. 04 ng / ml（ r 0. 999）; the average recovery was99. 5%. Conclution： The method is sample,accurate,reproducible and specific for determination of ethyl methanesulfonate in garenoxacin mesylate.