顶空气相色谱法测定苯磺酸贝他斯汀原料药中的残留溶剂

Determination of residue organic solvent in bepotastine besilate by headspace capillary gas chromatography

建立了气相色谱法测定苯磺酸贝他斯汀中残留溶剂含量的方法。采用HP-FFAP毛细管色谱柱(30 m×0.53 mm× 1.0 μm)和氢火焰离子化检测器(FID),并用程序升温方法进行测定。5种残留溶剂(丙酮、乙酸乙酯、二氯甲烷、乙醇、乙腈)均能完全分离,且在考察的浓度范围内线性关系良好(r大于0.995),回收率符合规定(平均回收率为98.1%~101.4%)。实验结果表明该气相色谱方法准确,灵敏度高,可用于苯磺酸贝他斯汀中残留溶剂的质量控制。

A gas chromatography method was established for the accurate and sensitive determination of five residual solvents such as acetone,ethyl acetate,dichloromethane,ethanol and acetonitrile in bepotastine besilate.An HP-FFAP capillary column and flame ionization detector were used with DMSO as the solvent.Five residual organic solvents were tested under a gradient temperature,and they were all separated effectively.The linearity was good(r >0.995)during the tested concentration range and the recovery also met the requirements of the determination(the average value of recovery was from 98.1%to 101.4%).The study results indicated the method was sensitive,accurate and can be used to supervise the residual solvents in bepotastine besilate.