顶空气相色谱法测定盐酸普拉克索中残留溶剂

Determination of Residual Organic Solvents in Pramipexole Hydrochloride Raw Materials by Headspace Gas Chromatography

目的：建立盐酸普拉克索中5种残留溶剂的测定方法。方法采用顶空进样毛细管气相色谱法, FID检测器,应用DB624毛细管柱,柱温采取程序升温,初始温度50℃,保持10 min,再以15℃·min-1的速率升至250℃,保持2 min,测定盐酸普拉克索原料药中乙醇、乙醚、二氯甲烷、乙酸乙酯和四氢呋喃的残留量。结果各有机溶剂均能得到有效分离,在所考察的浓度范围内线性关系良好,r为0.9979-0.9999,平均回收率为97.24%-102.24%（RSD为0.98%-1.82%,n=9）。结论本方法符合方法学验证要求,可用于盐酸普拉克索原料药中残留有机溶剂的检测。

Objective To establish a method for the content determination of the five residual organic solvents in Pramipexole Hydrochloride raw materials.Methods Headspace GC was adopted to determinate alcohol,ether,dichloromethane,ethyl acetate and tetramethylene oxide in Pramipexole Hydrochloride raw materials.FID detector, DB624 capillary column and programmable temperature were applied, the temperature was initially kept at 50 ℃ for 10 minutes,then raised to 250 ℃ at the rate of 15 ℃·min-1 and kept for 2 minutes.Results Five residual solvents were completely separated with good linear relationships （0.9979-0.9999）.The average recovery rates were in the range of 97.24%-102.24% （RSD0.98%-1.82%,n=9 ）.Conclusion The established method was in line with the requirements of methodology validation,which can be used for the quality control of the residual organic solvents in Pramipexole Hydrochloride raw materials.