气相色谱法测定他克莫司中的8种残留溶剂

目的用毛细管色谱柱气相方法建立他克莫司中有机残留溶剂的测定方法。方法采用DB-624(30m×0.53mm×3.0um)的毛细管柱;氢火焰离子化检测器(FID);柱温采用程序升温:初温45℃,保持4min后,以20℃/min升温至200℃,保持6min;载气为氮气,流速为4.1mL·min-1;进样口温度:170℃;检测器温度:250℃。结果 8种残留溶剂达到完全分离,在各自的浓度范围内具有良好的线性关系(所测试的8种溶剂的相关系数均为0.99以上),8种溶剂各个浓度的平均回收率在75.0%~150.0%,RSD小于10%。结论本方法简单,结果准确,可用于他克莫司多种残留溶剂的测定。

Determination of 8 kinds of resident solvents in tacrolimus by GC

OBJECTIVE To establish a method for the determination of residual organic sovents in Tacrolimus by capillary gas chromatography. METHODS DB-624 （30m x0.53mm x 3.0μm） was used as the capillary column with FID detection. The injector temperature was 170°C, and the detector temperature was 240°C, The initial column temperature was 45°C, maintaining it for 4 min, then raising the temperature to 200°C at the rate of 20°C / min, maintaining it for 6 min. Nitrogen was the carry gas. RESULTS Under the above condition, eight residual organic solvents were separated thoroughly, there was good linear relationship in the concentration range measured, The recoveries ranged was 75.0 %-150.0%, RSDs were not more than 10% respectively. CONCLUSION The method is proved to be simple and accurate. It is suitable for determination of organic solvents in Tacrolimus.