顶空毛细管气相色谱法测定盐酸莫西沙星中残留溶剂的含量

目的：建立盐酸莫西沙星中醋酸、乙酸乙酯、甲醇、乙醇、乙腈5种残留溶剂含量的测定方法。方法：顶空毛细管气相色谱法，氢火焰离子化检测器，醋酸以二甲基亚砜为溶剂，色谱柱为DB-FFAP（0．25mm×30m，0．25μm）；乙酸乙酯、甲醇、乙醇、乙腈以水为溶剂，异丙醇为内标，色谱柱为HP-INNOWax（0．32mm×30m，0．5μm）。结果：5种残留溶剂在对应于限度的20％～200％浓度范围内有良好的线性关系，平均回收率为97．3％～108．4％。结论：所建方法简单，准确，重现性好，可用于盐酸莫西沙星残留溶剂的含量控制。

HS-GC Determination of Residual Solvents in the Drug Substance of Moxifloxacin Hydrochloride

Objective： An HS-GC method was established for determination of residual solvents of acetic acid,ethyl acetate,methanol, ethanol,acetonitrile in the drug substance of moxifloxaein hydrochloride. Method： Acetic acid using DMSO as solvent, headspace gas chromatography was carried with DB-FFAP capillary column（0. 25 mm ×30 m, 0. 25 μm） and FID; ethyl acetate ,methanol ,ethanol, aeetonitrile using water as solvent and isopropanol as internal standard, headspace gas chromatography was carried with HP-INNOWax capillary column （0. 32 mm ×30 m, 0. 5μm） and FID. Results： The correlation coefficients of linearity ranged from 0. 9983 to 0. 9998 for the five residual solvents within the concentration of 20% to 200% of relative individual limit specified. Conclusion ： The method appears simple, accurate and reproducible. It can be applied to the quality control of residual solvent in the drug substance of moxifloxacin hydroehloride.