盐酸帕洛诺司琼中有机残留溶剂的检测  

Determination of the residual organic volatile solvents in palonosetron hydrochloride

作　　者：邓婕[1,2] 李志良[1,2] 肖玉梅 陈小勇 

机构地区：[1]重庆大学化学化工学院 [2]重庆人本药物研究院,重庆400041

出　　处：《药物分析杂志》2007年第5期735-737,共3页Chinese Journal of Pharmaceutical Analysis

基　　金：重庆直辖市应用基础基金(01-3-6);国家"春晖计划"教育部启动基金(99-4-4+37);霍英东基金资助(98-7-6);重庆大学自主创新科技攻关重点项目(03-5-6+04-10-10);重庆人本药物研究院(05-9-8)资助项目

摘　　要：目的:建立盐酸帕洛诺司琼中有机残留溶剂的检测方法。方法:毛细管气相色谱顶空进样法。色谱条件为:DM-624(30 m×0.53 mm,膜厚度为3.0 μm)毛细管柱;柱温为80℃;顶空进样瓶的平衡温度为80℃,平衡时间为80℃下平衡30min;进样口温度250℃,分流比:10:1;检测器温度250℃;载气:氮气;恒定压力,27 cm·s^(-1)(80℃);H_2流速:40 mL·min^(-1);空气流速:400 mL·min^(-1)。结果:3批样品中的有机溶剂残留量均符合要求。建立的色谱方法对待测溶剂具有良好的分离效果,在所考察的浓度范围内线性关系良好,各回收率均得到满意结果。结论:本方法操作简单,结果准确,是控制盐酸帕洛诺司琼中有机残留溶剂的可靠方法。Objective：To establish a headspace sampling GC method for the determination of the residual organic volatile solvents in palonosetron hydrochloride. Method：An Agilent DM -624 capillary column （30 m×0. 53 mm, 3.0μm） was used at 80℃ and programmed for 30 min. The temperatures of injection port and FI detector were 250 ~C ,10：1 of split ratio. Using nitrogen as the carrier gas at the invariable pressure of 27 cm ~ s-1. The flow rates were 40 mL ·min^-1 for H2 and 400 mL·min^-1 for the air. Results：The contents of residual solvents in three batches of samples were complied with the specific requirements. The linear ranges and the recoveries for residual solvents were satisfactory with good separation. Conclusion：The procedure provides a simple, rapid and sensitive method for monitoring residual solvents in palonosetron hydrochloride.

关 键 词：盐酸帕洛诺司琼 毛细管气相色谱 顶空进样 有机溶剂残留量 

分 类 号：R917[医药卫生—药物分析学]