顶空毛细管GC法测定匹多莫德原料药中6种溶剂的残留量

Determination of 6 kinds of residual solvents in pidotimod raw material by headspace capillary gas chromatography

目的:建立匹多莫德原料药中6种溶剂残留量的测定方法。方法:采用顶空毛细管气相色谱法,色谱柱为DB-624毛细管柱(30m×0.32mm,1.8μm),FID检测器,进样口温度为200℃,检测器温度为250℃;起始温度为60℃,维持5min,以20℃/min的速率升温至170℃,维持4min;顶空瓶平衡温度为80℃,平衡时间为15min。结果:在该色谱条件下,6种溶剂均能得到良好分离;6种溶剂的线性相关系数均大于0.999;精密度、重复性和稳定性试验的RSD均符合规定;6种溶剂的加样回收率均在92%~105%之间(RSD<10%,n=9)。结论:该方法操作简便,重复性高,结果稳定可靠,可用于匹多莫德残留溶剂的检测。

Objective: To detect the solvent residues in pidotimod raw material, we established a gas chromatography method for determination of 6 kinds of residual solvents. Methods: Headspace capillary gas chromatography was used with DB-624 capillary column(30 m×0.32 mm, 1.8 μm), and FID detector was used for solvent residues detection. The injector temperature was set at 200 ℃, and the detector temperature was set at 250 ℃. The initial column temperature was 60 ℃(maintained for 5 min), and the temperature was increased to 170 ℃(maintained for 4 min) at the rate of 20 ℃/min. The sample was extracted at 80 ℃ for 15 min. Results: Under above chromatographic conditions, all the six residual solvents were well separated, and the linear correlation coefficients of the six residual solvents were all greater than 0.999. RSD values of precision, repeatability and stability test were all in accordance with Pharmacopoeia requirements, and the recoveries of the six residual solvents were between 92% and 105%(RSD<10%, n=9). Conclusion: The established method is simple, reproducible, stable and reliable, and can be used for detection of residual solvents in pidotimod raw material.