顶空气相色谱法测定伊班膦酸钠中甲苯和氯苯的残留量

目的建立伊班膦酸钠原料药中有机溶剂甲苯和氯苯残留量检测的顶空气相色谱法。方法采用Agilent DB-624毛细管柱（30 m×0.53 mm,3μm）,程序升温方式,进样口温度180℃,检测器温度200℃,载气为N2,流速为5 mL/min,顶空瓶平衡温度为60℃,平衡时间为30 min。结果甲苯和氯苯分离良好,在所考察的质量浓度范围内具有良好的线性关系,r分别为0.999 3和0.999 4,平均回收率分别为90.96%和93.72%,精密度RSD均小于5%,最低检出质量浓度分别为0.35μg/mL和1.13μg/mL。3批样品中2种有机溶剂残留量均符合要求。结论所用方法简便快速、准确可靠,适于伊班膦酸钠原料药中有机溶剂残留量的检测。

Determination of Residual Quantity of Toluene and Chlorobenzene in Ibandronate Sodium by HS-GC

Objective To establish a headspace gas chromatography（HS-GC） method for quantitative determination of residual organic solvents in ibandronate sodium.Methods The chromatographic analysis was performed on the DB-624 capillary column（30 m × 0.53 mm,3 μm） with temperature programming,the injector temperature was set at 180 ℃,the FID detector was 200 ℃,and the elution rate of the carrier gas N2 was 5 mL/min.The headspace sampler vials was equilibrated at 60 ℃ for 30 min.Results Toluene and chlorobenzene were separated completely,and the linearity was good（r = 0.999 3,0.999 4）.The average recovery rates were 90.96% and 93.72%,and RSD was less than 5%.The detection limits were 0.35 μg/mL and 1.13 μg/mL,respectively.The content of two residual organic solvents in three batches of samples complied with the specification requirement.Conclusion The method is rapid,accurate and sensitive,which can be successfully used for the determination of toluene and chlorobenzene residuals in ibandronate sodium.