顶空GC法测定盐酸马普替林中6种残留溶剂  

Determination of 6 Residual Organic Solvents in Maprotiline Hydrochloride by Headspace GC

作　　者：王瑞芬 康鹏伟 WANG Rui-fen;KANG Peng-wei(Puyang Institute for Food and Drug Control,Puyang 457000,China;Puyang Institute for Food Supervision,Puyang 457000,China)

机构地区：[1]濮阳市食品药品检验检测中心,河南濮阳457000 [2]濮阳市食品监督所,河南濮阳457000

出　　处：《食品与药品》2023年第3期229-232,共4页Food and Drug

摘　　要：目的建立顶空气相色谱法测定盐酸马普替林原料药中6种有机溶剂的残留量。方法采用Agilent DB-624毛细管柱(30m×0.53mm,3.0μm)和氢火焰离子化检测器,程序升温,进样口温度220℃,检测器温度260℃,载气为高纯氮气,流速2.5 ml/min,顶空平衡温度80℃,平衡时间30 min。结果6种有机溶剂在各自质量浓度范围内与相应峰面积线性关系良好(r>0.9992);平均加样回收率为97.45%~100.13%,RSD为1.56%~2.38%。结论该方法操作简便、分析快捷、检测灵敏度高、结果准确,可用于盐酸马普替林原料药中6种有机溶剂残留量的测定。Objective To establish a headspace gas chromatography method for the determination of six residual solvents in maprotiline hydrochloride.Methods An Agilent DB-624 capillary column(30 m×0.53mm,3.0μm)with the FID detector was used for the determination.The programmed column temperature was set as follows:the temperature of the injector was 230℃and that of the FID was 250℃;the containers of headspace injector were in equilibrium at 80℃for 30 minutes,the carrier gas was nitrogen at a flow rate of 2.5 ml/min.Results There was a good linear relationship in the concentration ranges of 6 residual organic solvents with correlation coefficient above 0.9992,respectively.The average recoveries were 97.45%-100.13%,and the RSDs were 1.56%-2.38%.Conclusion The method is sample,rapid,sensitive,with accurate and reliable results,which can be applied in the ditermination of sixresidual solventsin maprotiline hydrochloride.

关 键 词：盐酸马普替林 残留溶剂 顶空气相色谱法 原料药 

分 类 号：O657.71[理学—分析化学] R927[理学—化学]