摘要
目的:采用顶空气相色谱法测定富马酸卢帕他定原料中的环己烷、乙酸乙酯、甲醇、二氯甲烷、三氯甲烷5种有机溶剂的残留量。方法:色谱柱:DB-WAXETRR毛细管色谱柱(30 m×0.32 mm,0.25μm);载气:氮气;FID检测器;进样口温度:200℃;采用程序升温:初始温度为35℃,保持10 min,以20℃·min^(-1)升温至220℃,保持5 min。结果:环己烷、乙酸乙酯、甲醇、二氯甲烷、三氯甲烷分别在77.590 1~698.310 9μg·ml^(-1)(r=0.999 7),102.166 6~919.499 4μg·ml^(-1)(r=0.999 8),62.744 7~564.703 2μg·ml^(-1)(r=0.999 9),12.011 2~108.101 1μg·ml^(-1)(r=0.999 6),1.262 8~11.365 6μg·ml^(-1)(r=0.999 6)范围内线性关系良好。5种残留溶剂的平均回收率分别为103.9%,103.5%,104.9%,107.1%,103.4%,RSD值分别为2.3%、2.6%、3.1%、2.8%、4.5%(n=9)。富马酸卢帕他定原料中均未检出此5种残留溶剂。结论:本方法稳定、简便、准确,灵敏度高,适用于富马酸卢帕他定原料中残留溶剂的测定。
Objective：To determine the content of cyclohexane,ethyl acetate,methanol,methylene chloride and trichloromethane in rupatadine fumarate by headspace gaschromatography.Methods：A DB-WAXETRR capillary column（30 m ×0.32 mm,0.25 μm） was used and the carrier gas was nitrogen.The detector was an FID and the inlet temperature was 200℃.The column temperature program was with the initial temperature of 35℃,maintained 10 min,and then risen to 220℃ with the rate of20℃ ·min^-1,and maintained 5 min.Results：Cyclohexane,ethyl acetate,methanol,methylene chloride and trichloromethane showed a good linear relationship within the range of 77.590 1-698.310 9 μg·ml^-1（r = 0.999 7）,102.166 6-919.499 4 μg·ml^-1（r = 0.999 8）,62.744 7-564.703 2μg·ml^-1（r = 0.999 9）,12.011 2^-108.101 1 μg·ml^-1（r = 0.999 6） and 1.262 8^-11.365 6 μg·ml^-1（r = 0.999 6）.The average recovery was 103.9%,103.5%,104.9%,107.1% and 103.4% and RSD was2.3%,2.6%,3.1%,2.8% and 4.5%（n = 9）,respectively.The five residual solvents were not detected out in rupatadine fumarate.Conclusion：The method is stable,simple,sensitive and accurate,and can be used for the determination of residual solvents in rupatadine fumarate.
出处
《中国药师》
CAS
2016年第5期1024-1026,共3页
China Pharmacist
关键词
富马酸卢帕他定
残留溶剂
顶空气相色谱法
Rupatadine fumarate
Residual solvents
Headspace gas chromatography
