毛细管气相色谱法测定多西他赛中的残留溶剂

Determination of Residual Solvents in Docetaxel by Capillary GC

目的:建立气相色谱法测定多西他赛原料药中残留溶剂的方法。方法:采用DB-FFAP弹性石英毛细管柱(30 m×0.32 mm×0.25μm);FID检测器;色谱条件:柱温40℃保持5.5 min,以20℃·min^(-1)的速率升温至220℃,保持5min;进样口温度为220℃;检测器温度为250℃;分流进样,分流比为1:20。结果:7种残留溶剂均呈现较好的线性关系(r=0.997 3～0.999 6);平均回收率为94.3%～111.7%。结论:本测定方法简便、准确,可用于多西他赛原料药溶剂残留量的控制。

Objective： To establish a Capillary GC method for determination the residual solvents in Docetaxel. Method： DB - FFAP capillary column（30 m × 0.32 mm × 0.25 μm） was used, the detector was FId, initial column temperature was kept at 40 ℃for 5.5 min, then rose to 220℃ with an increase rate of 20 ℃ min -1, and maintained for 5 min. Injector temperature was set at 220℃ and detector at 250 ℃ respectively. Split ratio was 1 ： 20. Result ： The calibration curves of residnal solvents in Docetaxel showed a good linearity（r = 0.9697 3 - 0. 999 6）, the average recovery was 94.3% - 111.7%. Conclusion ： The method is simple and accurate, it can be used for the control of the residual solvents in Docetaxel.