HS-GC法测定盐酸苯达莫司汀原料药中5种残留溶剂

Determination of 5 Residual Solvents in Bendamustine Hydrochloride API by HS-GC

目的建立顶空气相色谱法(HS-GC)测定盐酸苯达莫司汀中5种溶剂残留量。方法色谱柱为Agilent DB-624,流速1.0 mL/min;分流比10∶1;起始温度40℃,维持4 min,以30℃/min的速率升温至180℃,维持10 min;检测器为火焰离子化检测仪(FID);检测器温度250℃;进样口温度220℃;平衡温度80℃,平衡时间30 min。结果该方法可使5种残留溶剂得到有效分离,并在各自浓度范围内呈良好的线性关系(r>0.999);平均回收率94.57%~97.38%;各组份定量限分别为5.991,3.970,3.223,0.803,0.367μg/mL;各组份检测限分别为1.198,0.596,0.967,0.241,0.175μg/mL。结论该方法简便、准确,适用于盐酸苯达莫司汀中有机残留溶剂的检查。

Objective To establish a headspace gas chromatography(HS-GC)method for the determination of 5 solvent residues in bendamustine hydrochloride.Method The chromatographic column was Agilent DB-624,the flow rate was 1.0 mL/min;the split ratio was 10∶1;the starting temperature was 40℃and maintained for 4 minutes,and the temperature was increased to 180℃at a rate of 30℃/min and maintained for 10 minutes.The detector was FID and its temperature was 250℃.The inlet temperature was 220℃,the equilibrium temperature was 80℃,and the equilibrium time was 30 min.Results This method can effectively separate the five residual solvents and show a good linear relationship within their respective concentration ranges(r>0.999).The average recovery rate was 94.57%~97.38%.The quantification limits of each component were 5.99,3.970,3.223,0.803,0.367μg/mL.The detection limits of each component were 1.198,0.596,0.967,0.241μg/mL and 0.175μg/mL.Conclusion The method was simple,accurate,and suitable for the inspection of residual organic solvents in bendamustine hydrochloride.