论文部分内容阅读
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 method for the determination of residual solvent in docetaxel raw material by gas chromatography. Methods: DB-FFAP elastic quartz capillary column (30 m × 0.32 mm × 0.25 μm) was used. The FID detector was used. Chromatographic conditions: The column temperature was kept at 40 ℃ for 5.5 min and the temperature was increased to 20 ℃ · min -1 220 ° C for 5 min; inlet temperature 220 ° C; detector temperature 250 ° C; split injection, split ratio 1:20. Results: The seven residual solvents showed a good linear relationship (r = 0.997 3 to 0.999 6). The average recoveries ranged from 94.3% to 111.7%. Conclusion: The method is simple and accurate and can be used for the control of the residues of docetaxel API.