长沙理工大学学报（自然科学版）2016，Vol.13Issue(1)：93-98,6.
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
摘要
Abstract
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 ef-fective method for determining the residual amount of organic solvent was established.A headspace capillary GC with FID detector was selected to determine 5 kinds of organic as ac-etone,acetonitrile,dichloromethane,ethyl acetate and toluene.The determination was per-formed 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 a program of initial column temperature of 40 ℃,maintaining for 8 min,then raising to 240 ℃ at a rate of 20 ℃ /min,maintaining for 20 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 1 mL,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 0.61 6,6.72,4.89, 2.70,1.46 μg/mL,and the limits of quantitation(10S/N)were 1.85,1 6.8,13.9,8.07, 3.64 μg/mL,respectively.The recoveries of each solvent from standard addition were all in the range of 90%~1 10%.关键词
气相色谱法/顶空进样/雷贝拉唑钠/残留溶剂Key words
gas chromatography/headspace sampling/Rabeprazole sodium/residual solvent分类
化学化工引用本文复制引用
张玲,冯雪,谭淑珍,王述维,李浦江..顶空气相色谱法测定雷贝拉唑钠原料药中残留溶剂含量[J].长沙理工大学学报（自然科学版）,2016,13(1):93-98,6.基金项目
湖南省教育厅科研资助项目(14A012) （14A012）
