顶空气相色谱法同时测定盐酸金刚烷胺原料药中5种有机溶剂残留量  

Simultaneous determination of 5 residual organic solvents in amantadine hydrochloride by headspace GC

作　　者：王瑞芬 WANG Ruifen(Puyang Institute for Food and Drug Control,Puyang,He'nan 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

出　　处：《安徽医药》2024年第8期1529-1531,共3页Anhui Medical and Pharmaceutical Journal

摘　　要：目的建立顶空气相色谱法定量分析盐酸金刚烷胺原料药中乙醇、丙酮、乙腈、二氯甲烷和三氯乙烷残留量方法。方法采用Agilent DB-624色谱柱(30 m×0.53 mm,3.0μm),程序升温,FID检测器,进样口温度200℃,检测器温度250℃,载气为氮气(N_(2)),流速2.5 mL/min,分流比5∶1,顶空平衡温度80℃,平衡时间30 min。结果有机溶剂浓度与峰面积相关性系数大于0.9993;加样回收率97.78%~101.03%,相对标准偏差(RSD)1.27%~2.26%。结论该分析方法高效快捷、重复性与稳定性好,准确度高,有望为盐酸金刚烷胺原料药中乙醇、丙酮、乙腈、二氯甲烷和三氯乙烷残留溶剂的定量分析控制提供扎实的试验依据。Objective To establish a headspace gas chromatography method for quantitative analysis of residual amounts of ethanol,acetone,acetonitrile,dichloromethane,and trichloroethane in amantadine hydrochloride raw materials.Methods The separation used Agilent DB-624 capillary column(30 m×0.53 mm,3.0μm),programmed heating,FID detector.The inlet temperature and the detector temperature were set at 200℃and 250℃,respectively.Carrier gas was nitrogen(N_(2)),the flow rate was 2.5 mL/min,the split ratio was 5∶1,and the headspace equilibrium temperature was 80℃.Balance time was 30 min.Results There was a good linear relationship between the concentration of the solvent to be tested and its peak area(correlation coefficient>0.9993);The average sample recovery rate is 97.78%to 101.03%,and the RSD was 1.27%to 2.26%.Conclusions This analytical method is efficient,fast,with good repeat⁃ability and stability,and high accuracy.It is expected to provide a solid experimental basis for the quantitative analysis and control of residual solvents such as ethanol,acetone,acetonitrile,dichloromethane,and trichloroethane in amantadine hydrochloride raw materials.

关 键 词：金刚烷胺 有机溶剂残留 气相色谱 原料药 

分 类 号：R927.2[医药卫生—药学]