气相色谱-质谱法测定盐酸雷尼替丁中基因毒性杂质

Determination of genotoxic impurity in ranitidine by GC-MS

目的:建立一种测定盐酸雷尼替丁中基因毒性杂质呋喃甲醇的气相色谱-质谱联用方法。方法:采用毛细管柱TG-1701MS(30 m×0.25 mm,0.25μm),程序升温,初始温度为50℃,维持2 min,以15℃·min^-1的速率升温至110℃,维持2 min;再以20℃·min^-1的速率升温至210℃,维持2 min,以氦气为载气,流速为1 mL·min^-1,采用电子轰击离子化离子源(EI),在选择离子监测模式(SIM)下对m/z 98离子进行选择性监测。结果:呋喃甲醇在0.169~0.948μg·mL^-1浓度范围内线性关系良好,定量限为169.27 ng·mL^-1,检测限为50.78 ng·mL^-1,平均回收率为101.2%。结论:本法操作简单、准确、专属性强且重现性好,适用于盐酸雷尼替丁中基因毒性杂质呋喃甲醇的检测。

Objective:To establish a GC-MS analytical method for the determination of furfuryl alcohol in ranitidine.Methods:The analytical column was Thermo TG-1701MS(30 m×0.25 mm,0.25μm).The column temperature was maintained at 50℃for 2 min,then was raised to 110℃at the rate of 15℃·min^-1.After being maintained at 110℃for 2 min,the temperature was raised to 210℃at the rate of 20℃·min^-1 and was maintained at 210℃for 2 min.Helium was used as carrier gas,and its flow rate was 1.0 mL·min^-1.The detection was achieved by EI-MS,and the selective ion monitor was set at m/z 98 in SIM mode.Results:The calibration curve of furfuryl alcohol had good linearity in the concentration range of 0.169~0.948μg·mL^-1.The limits of quantification and detection were 169.27 and 50.78 ng·mL^-1,respectively.The repeatability of this method was fine with RSD value of 5.8%.In addition,the average recovery of the three spiked concentrations of furfuryl alcohol was 101.2%.The specificity of this method was good for determining furfuryl alcohol in ranitidine.Furfuryl alcohol was not detected in three batches of ranitidine samples.Conclusion:The established method showed satisfactory convenience,accuracy,specificity and repeatability.This method could be used for determination of furfuryl alcohol in ranitidine.