顶空气相色谱法测定雷贝拉唑钠原料药中残留溶剂含量  

Determination of residual solvents in rabeprazole sodium raw material by headspace gas chromatography

作　　者：张玲[1] 冯雪[1] 谭淑珍[1] 王述维 李浦江 

机构地区：[1]长沙理工大学化学与生物工程学院,湖南长沙410004 [2]湖南如虹制药有限公司,湖南岳阳414300

出　　处：《长沙理工大学学报（自然科学版）》2016年第1期93-98,共6页Journal of Changsha University of Science and Technology:Natural Science

基　　金：湖南省教育厅科研资助项目(14A012)

摘　　要：利用气相色谱法测定雷贝拉唑钠原料药中丙酮、乙腈、二氯甲烷、乙酸乙酯和甲苯5种有机溶剂残留量,通过优化实验条件建立了一种有效的测定有机溶剂残留量的方法。采用顶空毛细管气相色谱法,检测器为氢火焰离子化检测器,色谱柱为DB-624石英毛细管柱,以氮气为载气,流速为2.0mL/min;柱温采取程序升温方式,于40℃保持8min,然后以每分钟20℃的速率升温至240℃,并保持20min;顶空平衡温度为90℃,平衡时间为30min;进样口温度为200℃,检测温度为250℃;进样体积为1mL,分流比为5∶1。5种有机溶剂在该色谱条件下均能有效分离,峰面积与浓度呈现良好的线性关系,相关系数R圴大于0.990,检出限（3S/N）分别为0.616,6.72,4.89,2.70,1.46μg/mL,定量限（10S/N）分别为1.85,16.8,13.9,8.07,3.64μg/mL,各残留溶剂的加标回收率均在90%~110%范围内。A gas chromatography（GC）method was developed for the determination of five residual solvents including acetone,acetonitrile,dichloromethane,ethyl acetate and toluene in rabeprazole sodium raw material.Based on the optimized experimental conditions,an effective method for determining the residual amount of organic solvent was established.A headspace capillary GC with FID detector was selected to determine 5kinds of organic as acetone,acetonitrile,dichloromethane,ethyl acetate and toluene.The determination was performed on DB-624 capillary column with nitrogen gas as carrier gas at the rate of 2.0 mL/min.The column temperature was controlled by aprogram of initial column temperature of40 ℃,maintaining for 8min,then raising to 240 ℃ at a rate of 20 ℃ /min,maintaining for20 min.The headspace equilibrium temperature was 90℃and equilibrium time was 30 min.The temperature of the injector was maintaining at 200 ℃ and that of detector at 250 ℃.The injection volume of sample was 1mL,and the split ratio was 5：1.The five residual sol-vents were separated completely under given chromatogram systems.The calibration curve of each solvent showed a good linear relationship,and the correlation coefficients（R）of each solvent is more than 0.990.The limits of detection（3S/N）were 0.616,6.72,4.89,2.70,1.46μg/mL,and the limits of quantitation（10S/N）were 1.85,16.8,13.9,8.07,3.64μg/mL,respectively.The recoveries of each solvent from standard addition were all in the range of 90%~110%.

关 键 词：气相色谱法 顶空进样 雷贝拉唑钠 残留溶剂 

分 类 号：O657.7[理学—分析化学]