顶空毛细管气相色谱法测定盐酸萘甲唑啉有机溶剂残留量

Determination of residual organic solvents in naphzoline hydrochloride by headspace capillary gas chromatography

建立顶空毛细管气相色谱法测定盐酸萘甲唑啉中两种残留溶剂的含量。采用DB-624毛细管色谱柱(30 m×0.320 mm,1.80μm);程序升温,载气为高纯氮气,流速为2.0 mL/min;氢火焰离子化检测器,检测器温度220℃;进样口温度180℃;顶空进样,平衡温度80℃,平衡时间20 min。结果表明:残留溶剂乙醇和丙酮完全分离,乙醇和丙酮浓度分别在0.1004~0.9036 mg/mL和0.1013~0.9117 mg/mL范围内线性关系良好(r^(2)≥0.9998);平均回收率分别为100.4%和99.8%,RSD分别为0.7%和0.5%(n=9)。该方法准确,简便,灵敏度高,重复性好,适用于盐酸萘甲唑啉残留溶剂的含量测定。

To establish a method for determination of two residual solvents in naphthozoline hydrochloride by headspace capillary gas chromatography.The analysis was performed on DB-624 capillary column(30 m×0.320 mm,1.80μm);The column temperature program was raised and the high purity nitrogen was used as the carrier gas with the flow rate of 2.0 mL·min^(-1);The FID detector temperature and the injector temperature were respectively set at 220℃and 180℃.The containers of headspace injector were in equilibrium for 20 min at 80℃.The result showed that the residual solvent ethanol and acetone were separated completely.The linear range of ethanol and acetone were 0.1004-0.9036 mg·mL^(-1) and 0.1013-0.9117 mg·mL^(-1)(r^(2)≥0.9998),respectively.The average recoveries(n=9)were 100.4%and 99.8%,withRSDs were 0.7%and 0.5%,respectively.The method suitable for the determination of naphthozoline hydrochloride residual solvent is accurate,simple,highly sensitive and repeatable.