气相色谱法测定盐酸萘甲唑啉原料药中7种残留溶剂

Determination of Seven Residual Solvents in Naphthalmezoline Hydrochloride by GC

目的:建立气相色谱法测定盐酸萘甲唑啉原料药残留溶剂。方法:气相色谱法采用聚乙二醇为固定液的毛细管柱,规格30 m×0.32 mm×0.5μm,程序升温:起始温度为50℃,维持13 min,以20℃/min的速率升温至200℃,维持3 min。进样口温度:200℃;FID检测器温度:250℃;顶空瓶平衡温度:90℃,平衡时间为30 min;分流比:35∶1;载气:氮气;平均线速度:20 cm/s。结果在选定的条件下,空白无干扰且各残留溶剂峰分离度良好;乙醚、丙酮、乙酸乙酯、甲醇、异丙醇、乙醇、苯分别在LOQ~150%浓度范围内线性关系良好。检测限浓度依次为0.26×10^(-3),0.0124,8.01×10^(-3),0.227,0.05,0.128,3.16×10^(-3)μg/mL;定量限浓度依次为0.519×10^(-3),0.0373,0.0267,0.682,0.149,0.255,9.49×10^(-3)μg/mL;重复性和回收率结果良好。结论:该法专属、准确、易于操作,适用于盐酸萘甲唑林残留溶剂的测定。

Objective To establish a gas chromatography method for the determination of residual solvent of Naphthalmezoline Hydrochloride API.Methods Gas chromatography was performed on a capillary column with polyethylene glycol as the fixed solution,the size of which was 30 m×0.32 mm×0.5μm.The temperature was programmed:the initial temperature was 50℃,maintained for 13 min,and the temperature was raised to 200℃at a rate of 20℃/min,maintained for 3 min.Inlet temperature:200℃;FID detector temperature:250℃;Balance temperature of headspace bottle:90℃,balance time:30 min;Shunt ratio:35∶1;Carrier gas:Nitrogen;Average linear speed:20 cm/s.Results Under the selected conditions,there is no interference in the blank and the separation degree of each residual solvent peak is good.The linear relationship of ethyl ether,acetone,ethyl acetate,methanol,isopropanol,ethanol and benzene was good in the concentration range of LOQ~150%.The LOD were 0.26×10^(-3),0.0124,8.01×10^(-3),0.227,0.05,0.128,3.16×10^(-3)μg/mL,respectively.The LOQ were 0.519×10^(-3),0.0373,0.0267,0.682,0.149,0.255,9.49×10^(-3)μg/mL,respectively.The results of reproducibility and recovery were good.Conclusion:The method is exclusive,accurate and easy to operate.It is suitable for the determination of residual solvent of naphthalmezolin hydrochloride.