顶空毛细管气相色谱法测定盐酸格拉司琼中残留溶剂

目的:建立顶空气相色谱法测定盐酸格拉司琼中两种残留溶剂四氢呋喃、甲醇的含量。方法:以水为溶解介质,丙酮为内标物,采用HP-INNOWAX毛细管柱,程序升温,氢火焰离子化检测器检测;顶空平衡温度为80℃,顶空平衡时间为30min,进样时间为1.0 min。结果:四氢呋喃在0.11～12.80μg·ml^-1（r=0.999 3）、12.80～28.43μg·ml^-1（r=0.999 9）,甲醇在0.48～15.83μg·ml^-1（r=0.999 0）、15.83～142.50μg·ml^-1（r=0.999 7）范围内线性良好;四氢呋喃的高中低加样回收率分别为89.4%～92.4%,87.9%～91.8%,86.5%～89.3%;甲醇的高中低加样回收率分别为98.4%～101.6%,98.1%～103.6%,97.7%～102.8%。结论:该方法可用于盐酸格拉司琼残留溶剂测定。

Determination of Residual Organic Solvents in Granisetron Hydrochloride by Headspace Capillary Gas Chromatography

Objective： To establish a method for determining two residual organic solvents （tetrahydrofuran and methanol） in granisetron hydrochloride by headspace capillary gas chromatography. Method： The HP-INNOWAX capillary column was used. Sample was dissolved in water, and acetone was employed as the internal standard. FID detector was used under programmed column temperature control, and equilibrium temperature was 80 ℃, equilibrium time was 30 min and injection time was 1.0 min. Result： The standard curves were linear within the range of 0. 11-12. 80μg·ml^-1 （ r = 0. 999 3 ） and 12. 80-28.43 μg·ml^-1 （ r = 0. 999 9 ） for tetrahydrofuran, 0. 48-15.83 μg·ml^-1 （r =0. 999 0） and 15.83-142. 50 μg·ml^-1 （r =0. 999 7） for methanol. Average recovery of high, medium and low concentration of tetrahydrofuran was between 89. 4% -92. 4%, 87.9% -91.8%, and 86. 5% -89. 3%, respectively. For methanol, it was between 98.4% -101.6% ,98.1% -103.6%, and 97. 7% -102. 8%, respectivly. Conclusion： This method can be used for determination of residual organic solvents in granisetron hydrochloride.