顶空气相色谱法测定福沙匹坦二甲葡胺中8种残留溶剂的含量

目的:建立顶空气相色谱法测定福沙匹坦二甲葡胺中甲醇、乙醇、丙酮、乙腈、甲基叔丁基醚、四氢呋喃、乙酸乙酯及甲苯残留量的方法。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45℃,维持5 min,再以20℃·min^-1的速率升温至200℃,维持3 min。顶空平衡温度为80℃,平衡时间为20 min。结果:8种残留溶剂分离度良好,在一定浓度范围内呈良好的线性关系(r≥0.9997),平均回收率在95%~105%范围内,检出限分别为0.19,0.31,0.06,0.13,0.03,0.05,0.16,0.12μg·ml^-1。结论:该方法灵敏度高,准确度好,适用于福沙匹坦二甲葡胺原料药中残留溶剂的测定。

Determination of 8 Residual Solvents in Fosaprepitantdimeglumine by Headspace Gas Chromatography

Objective:To establish a headspace gas chromatography method for the determination of methanol,ethanol,acetone,acetonitrile,methyl-butyl ether,tetrahydrofuran,ethyl acetate and methylbenzene in fosaprepitantdimeglumine.Methods:A headspace gas chromatography method was used to separate the residual solvents on a DB-624 capillary column(30 m×0.53 mm,3.0μm).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 with the temperature at 250℃.The column temperature program was with the initial temperature of 45℃(maintaining 5 min),and up to 200℃at the rate of 20℃·min^-1(maintaining 3 min).The containers of headspace injector were in equilibrium at 80℃for 20 min.Results:The 8 solvents were well separated.There were good linear relationships,and the correlation coefficients were no less than 0.9997.The average recovery was within the range of 95%-105%.The limit of detection was 0.19,0.31,0.06,0.13,0.03,0.05,0.16 and 0.12μg·ml^-1,respectively.Conclusion:The established method is sensitive and accurate,and suitable for the determination of residual solvents in fosaprepitantdimeglumine.