顶空气相色谱法测定枸橼酸托瑞米芬原料药中溶剂残留量

目的:建立测定枸橼酸托瑞米芬原料药中4种溶剂(丙酮、四氢呋喃、乙酸乙酯和甲苯)残留量的方法。方法:采用顶空气相色谱法。以二甲亚砜为溶剂,苯为内标物,色谱柱为HP-INNOWAX毛细管柱,程序升温,氢火焰离子化检测器,顶空平衡温度90℃、顶空平衡时间20min、进样时间1.0min。结果:丙酮、四氢呋喃、乙酸乙酯、甲苯检测浓度线性范围分别为1.264～31.59、0.8886～22.22、1.621～40.52、1.732～43.30μg·mL-1(r均>0.9994);回收率分别为98.74%～102.0%、99.22%～100.6%、98.86%～100.8%、98.72%～101.9%;RSD分别为1.9%、2.3%、1.7%、1.9%(n=7);检出限分别为0.1154、0.3550、0.1054、0.1303μg·mL-1,样品中4种溶剂残留量均符合《中国药典》规定。结论:所建立的方法可用于枸橼酸托瑞米芬原料药中溶剂残留量的测定。

Content Determination of Residual Organic Solvents in Toremifene Citrate by Headspace Gas Chromatography

OBJECTIVE：To the method for the content determination of 4 kinds of residual organic solvents in toremifene citrate,such as acetone,tetrahydrofuran,ethyl acetate and toluene.METHODS：Headspace gas chromatography was adopted using dimethyl sulfoxide as solvent and benzene as internal standard.HP-INNOWAX capillary column was used.FID detector was used under programmed column temperature control.Equilibrium temperature was 90℃,equilibrium time was 20 min and injection time was 1.0 min.RESULTS：The linear ranges were 1.264～31.59μg·mL -1 （r0.999 4）for acetone,0.888 6～22.22μg·mL -1 （r0.999 4）for tetrahydrofuran,1.621～40.52μg·mL -1 （r0.999 4）for ethyl acetate and 1.732～43.30μg·mL -1 （r0.999 4） for toluene.The recoveries were between 98.74%～102.0%,99.22%～100.6%,98.86%～100.8%,98.72%～101.9%,respectively.RSD（n=7）were 1.9%,2.3%,1.7%,1.9% respectively.The detection limits were 0.115 4μg·mL -1 ,0.355 0μg·mL -1 , 0.105 4μg·mL -1 ,0.130 3μg·mL -1 ,respectively.CONCLUSION：This method can be used for the determination of residual organic solvents in toremifene citrate.