顶空气相色谱法测定依折麦布中5种残留溶剂的含量

Determination of 5 Residual Solvents in Ezetimibe by Headspace Gas Chromatography

目的:建立顶空气相色谱法测定依折麦布中异丙醇、二氯甲烷、甲基叔丁基醚、正己烷及乙酸乙酯的残留量的方法。方法:采用顶空气相色谱法,色谱柱为DB-624毛细管柱(30 m×0.53 mm,3.0μm),载气为氮气,流速为2.0 ml·min^(-1),进样口温度为200℃,FID检测器,检测器温度为250℃,程序升温:起始温度为35℃,以10℃·min^(-1)的速率升温至85℃,再以25℃·min^(-1)的速率升温至210℃,维持3 min。顶空平衡温度为90℃,平衡时间为20 min。结果:5种残留溶剂分离度良好,线性关系良好(r≥0.999 6),平均回收率在95%~105%范围内(n=9),检出限分别为0.07,0.24,0.07,0.01,0.07μg·ml^(-1)。结论:该方法灵敏度高,准确度好,适用于依折麦布原料药中残留溶剂的测定。

Objective:To establish a headspace gas chromatography method for the determination of isoproanol,methylene chloride,methyl-butyl ether,n-hexane and ethyl acetate in ezetimibe.Methods:A headspace gas chromatography method was used to separate the residual solvents on a DB-624 capillary column(30 m×0.53 mm,3.0 μm).The carrier gas was nitrogen.The flow rate was 2.0 ml·min^(-1).The temperature of injector was 200℃.A flame ionization detector was used at the temperature of 250℃.The column temperature program was at the initial temperature of 35℃,risen to 85℃ at the rate of 10℃·min^(-1),and risen to 210℃ at the rate of 25℃·min^(-1)( maintaining 3 min).The containers of headspace injector were in equilibrium at 90℃ for 20 min.Results:The 5 solvents were well separated.There were good linear relationships,and the correlation coefficients were not lower than 0.999 6.The average recoveries were within the range of 95%-105%(n=9).The limit of detection was 0.07,0.24,0.07,0.01 and 0.07 μg·ml^(-1),respectively.Conclusion:The established method is sensitive and accurate,and suitable for the determination of residual solvents in ezetimibe.