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顶空气相色谱法测定盐酸格拉司琼中多种有机溶剂残留量
Determination of Residual Solvent in Granisetron Hydrochloride by Headspace Gas Chromatography
【摘要】 建立盐酸格拉司琼原料中多种有机溶剂残留量的分离测定方法。采用顶空气相色谱法,载气为氮气,FID检测器,色谱柱为HP-1毛细管柱,程序升温,外标法测定盐酸格拉司琼中甲醇、异丙醇、乙醚、二氯甲烷、氯仿、四氢呋喃、二甲基甲酰胺、甲苯的残留量。8种有机溶剂完全分离,在所考察的浓度范围内具有良好的线性,r为0.9988~0.9997,平均回收率为93.5%~103.1%,精密度RSD均小于10%,检测限为0.003~1.15μg.ml-1。本方法快速、灵敏、准确,适用于盐酸格拉司琼中多种有机溶剂残留量的测定。
【Abstract】 A headspace gas chromatography method for separating and determining various kinds of residual organic solvents in granisetron hydrochloride was established.A HP-1 capillary column was used with nitrogen gas as carrier and FID as detector.The organic residuals including methanol,isopropanol,ethyl ether,dichloromethane,chloroform,tetrahydrofuran,N,N-dimethylformamide and toluene were separated and determined.There was good linearity(r =0.99880.9997).The average recovery rates were within the range of 93.5% and 103.1%,and each RSD was less than 10%.The detection limits were within 0.003 1.15μg·ml-1.The method was rapid,sensitive and accurate. It could be used for the determination of various organic residuals in granisetron hydrochloride.
【Key words】 Granisetron Hydrochlorofome; residual solvent; headspace gas chromatography;
- 【文献出处】 中国药事 ,Chinese Pharmaceutical Affairs , 编辑部邮箱 ,2006年08期
- 【分类号】R927
- 【被引频次】9
- 【下载频次】87