顶空气相色谱法测定盐酸帕罗西汀中残留的有机溶剂及基质效应考察  

Determination of residual organic solvents in paroxetine hydrochloride by headspace capillary GC and research of matrix-induced effect

作　　者：孙悦[1] 王卫[1] 唐素芳[1] 

机构地区：[1]天津市药品检验所,天津300070

出　　处：《药物分析杂志》2010年第5期963-967,共5页Chinese Journal of Pharmaceutical Analysis

基　　金：中国药典2010年版科研课题项目

摘　　要：目的:建立盐酸帕罗西汀中6种残留有机溶剂的分离测定方法,考察盐酸帕罗西汀的基质效应。方法:采用顶空进样毛细管气相色谱法,应用DB-624石英毛细管柱(0.32mm×30m,1.80μm),载气为氮气,氢火焰离子化检测器(FID),程序升温,柱温50℃,保持10min,以6℃.min-1的速度升至80℃,保持5min,再以40℃.min-1的速度升至150℃,保持5min。采用方差分析方法对不同量的盐酸帕罗西汀产生的基质效应进行统计分析。结果:6种有机溶剂均能得到有效分离,在所考察的浓度范围内线性关系良好,r为0.9997～0.9999,平均回收率为99.1%～102.0%。不同量的盐酸帕罗西汀产生的基质效应有非常显著性差异(p<0.01)。结论:本方法灵敏、简便快速、结果准确,可用于盐酸帕罗西汀中残留有机溶剂的检测,基质效应差异显著。Objective：To establish GC method for determining the residual organic solvents in paroxetine hydrochloride and review the matric-induced effect of paroxetine hydrochloride.Methods：The six organic solvents were determined by headspace capillary GC and separated on a DB-624 capillary column（0.32 mm×30 m,1.80 μm）,with FID detector,nitrogen as the carry gas.The programmed column temperature was set as follows：maintained at 50 ℃ for 10 min and then raised to 80 ℃ at the rate of 6 ℃·min-1 follow by holding for 5 min,and raised to 150 ℃ at the rate of 40 ℃·min-1 follow by holding for 5 min.Matric-induced effect of paroxetine hydrochloride were calculated and analyzed by statistical method.Results：Six residual organic solvents were completely separated and there were good linearies （r=0.9997-0.9999）.The average recovery rate was in the range of 99.1%-102.0%.Matric-induced effect of paroxetine hydrochloride has remarkable difference（p0.01）.Conclusion：The methods is accurate and sensitive after validation and can be used for the determination of residual solvents in paroxetine hydrochloride and remarkable difference has be found in matric-induced effect of paroxetine hydrochloride.

关 键 词：顶空气相色谱法 盐酸帕罗西汀 残留有机溶剂 基质效应 

分 类 号：R917[医药卫生—药物分析学]