毛细管气相色谱法同时测定盐酸替利定原料药中4种有机溶剂残留量

目的:建立了以毛细管气相色谱法同时测定盐酸替利定原料药中丙酮、乙酸乙酯、四氢呋喃、甲苯4种有机溶剂残留量的方法。方法:色谱条件为DB-1701毛细管柱,氢火焰离子化检测器,检测器温度为250℃,柱温采用程序升温,初始温度为35℃,保持8min,以30℃·min-1升至180℃,保持2min,进样口温度为155℃,载气为氮气,流速为0.7mL·min-1,分流比为15∶1,进样量为1μL;以二甲基甲酰胺为溶剂。结果:丙酮、乙酸乙酯、四氢呋喃、甲苯的检测浓度线性范围分别为0.100～1.000、0.100～1.000、0.018～0.144、0.0178～0.178mg·mL-1(r为0.9993～0.9999),平均加样回收率为98.2%～99.5%,RSD小于1.5%。3批样品中乙酸乙酯均未检出,丙酮、四氢呋喃、甲苯残留量均符合《中国药典》2005年版要求。结论:本法快速、灵敏、准确,适用于盐酸替利定原料药中有机溶剂残留量的测定。

Determination of 4 Kinds of Residual Organic Solvents in Tilidine Hydrochloride by Capillary GC

OBJECTIVE： To establish capillary GC for the content determination of residual organic solvents （acetone, ethyl acetate, tetrahydrofuran and toluene） in tilidine hydrochloride. METHODS： DB-1701 capillary column was used with FID as detector. The temperature of detector was set at 250 ℃ and temperature programming of column was adopted. The initial temperature of column was at 35 ℃ for 8 min and increased to 180 ℃ at rate of 30 ℃·min^-1 for 2 min. The temperature of injection was 155 ℃ and nitrogen was used as carrier at flow rate of 0.7 mL·min^-1. Split ratio was 15 ∶ 1 and injection volume was 1 μL. DMF was used as solvent. RESULTS： The linear ranges were 0.100～1.000 mg·mL^-1 for acetone, 0.100～1.000 mg·mL^-1 for ethyl acetate, 0.018～0.144 mg·mL^-1 for tetrahydrofuran and 0.017 8～0.178 mg·mL^-1 for toluene （r=0.999 3～0.999 9）. Average recoveries were 98.2%～99.5% and RSD1.5%. Ethyl acetate hadn’t been found in 3 batches of samples, and acetone, tetrahydrofuran and toluene were all in line with the requirement of Chinese Pharmacopeia （2005 edition）. CONCLUSIONS： The method is rapid, sensitive and accurate. It is suitable for the content determination of residual organic solvents in tilidine hydrochloride.