顶空气相色谱法同时测定比沙可啶原料药中2种溶剂残留量-中国药房.PDF

顶空气相色谱法同时测定比沙可啶原料药中2种溶剂残留量 ＊ 姜建国 ，孙 婷，郭永辉，韩学静，苗会娟（河北省药品检验研究院，石家庄 050011） 中图分类号 R917 文献标志码 A 文章编号 1001-0408（2016）30-4297-03 DOI 10.6039/j.issn. 1001-0408.2016.30.39 摘 要 目的：建立同时测定比沙可啶原料药中二氯甲烷和乙酸乙酯残留量的方法。方法 ：采用顶空气相色谱法。色谱柱为以 6％氰丙基苯基-94％二甲基聚硅氧烷（DB-624）为固定液的毛细管柱，程序升温，进样口温度为220 ℃，检测器为氢火焰离子化检 测器，温度为250 ℃，载气为高纯氮气，载气流速为3.0ml/min ，分流比为1∶10，顶空加热温度为70℃，平衡时间为30min ，顶空瓶 装样量为5ml ，顶空进样量为1ml 。结果：二氯甲烷和乙酸乙酯检测质量浓度线性范围分别为6～120μg/ml （r ＝0.9999）、 50～1000μg/ml （r ＝0.9999）；定量限分别为0.2、1.7μg ，检测限分别为0.06、0.5μg ；精密度、稳定性、重复性试验的RSD ≤3％；加 样回收率分别为100.30％～102.00％（RSD ＝0.63％，n ＝9）、100.10％～101.30％（RSD ＝0.44％，n ＝9）。结论：该方法操作简便、结 果准确，可用于同时测定比沙可啶原料药中二氯甲烷和乙酸乙酯的残留量。 关键词 比沙可啶；顶空气相色谱法；溶剂残留量；二氯甲烷；乙酸乙酯 Simultaneous Residual Determination of Two Organic Solvents in Bisacodyl Raw Material by Head-space GC JIANG Jianguo ，SUN Ting ，GUO Yonghui ，HAN Xuejing ，MIAO Huijuan （Hebei Institute for Drug Control ，Shiji- azhuang 050011，China ） ABSTRACT OBJECTIVE ：To establish a method for simultaneous residual determination of dichloromethane and ethyl acetate in bisacodyl raw material. METHODS ：Head-space GC was performed on the capillary column of 6％ cyanopropyl phenyl-94％ di- methyl polysiloxane （DB-624）by temperature programming ，the temperature of injector was 220 ℃，detector was flame ionization detector with temperature of 250 ℃，carrier gas was high purity nitrogen with the flow rate of 3.0 ml/min ，split ration was 1∶10， headspace heating temperature was 70 ℃，equilibration time was 30 min ，volume of headspace vial was 5 ml ，and the injection volume was 1ml. RESULTS ：The linear range was 6-120μg/ml for dichloromethane （r ＝0.999 9）and 50-1000 μg/ml for ethyl ac- etate （r ＝0.999 9）；the limit of quantitation was 0.2，1.7 μg ，limit of detection was 0.06，0.5 μg ；RSDs of precision ，stability and reproducibility tests were no higher than 3％；recoveries were 100.30％-102.00％ （RSD ＝0.63％，n ＝9）and 100.10 ％-101.30％