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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。
Objective: To establish a method for the determination of two residual solvents, tetrahydrofuran and methanol, in granisetron hydrochloride by headspace gas chromatography. Methods: With water as the dissolution medium and acetone as the internal standard, HP-INNOWAX capillary column was used to program temperature and hydrogen flame ionization detector. The equilibrium temperature of headspace was 80 ℃, the equilibrium time of headspace was 30 min, For 1.0 min. Results: The results showed that the molar ratio of tetrahydrofuran in the range of 0.11-12.80μg · ml -1 (r = 0.999 3), 12.80-28.43μg · ml -1 (r = 0.999 9) and 0.48-15.83μg · ml -1 -1) (r = 0.999 0) and linear range of 15.83-142.50 μg · ml -1 (r = 0.999 7). The recoveries of high, middle and low tetrahydrofuran samples were 89.4% -92.4%, 87.9% ~ 91.8% and 86.5% ~ 89.3%, respectively. The high, medium and low recoveries of methanol were 98.4% ~ 101.6%, 98.1% ~ 103.6% and 97.7% ~ 102.8%, respectively. Conclusion: This method can be used for the determination of granisetron hydrochloride residual solvent.