顶空气相色谱法测定氟哌啶醇中有机溶剂残留量

Determination of Residual Solvents in Haloperidol by Headspace Gas Chromatography

目的建立测定氟哌啶醇中有机溶剂残留量的顶空气相色谱法。方法采用顶空气相色谱法,FID检测器,在毛细管色谱柱HP-Innowax毛细管柱(30 m×0.32 mm,0.50μm)上程序升温,载气为氮气,进样口温度为200℃,检测器温度为250℃。结果甲苯和乙醇分离良好,在所考察的质量浓度范围内具有良好线性关系,最低检出质量浓度分别为0.222 2μg/mL和0.197 3μg/mL,精密度的RSD分别为2.2%和2.0%(n=5),平均回收率分别为101.8%和100.6%,RSD分别为2.2%和1.2%(n=6)。结论该方法简便灵敏、结果准确可靠,适用于氟哌啶醇原料药中有机溶剂残留量的检测。

Abstract： Objective To establish a method for determining the residual solvents in haloperidol by headspace gas chromatogra- phy. Methods The determination was carried out on the HP- Innowax capillary column （30m×0.32mm,0.50μm） with sequential increase of temperature programming. The carrier gas was nitrogen, the injector temperature was 200 ℃ , and the FID detector tempera- ture was 250 ℃. Results The residual solvents toluene and ethanol were well separated. The good linearity appeared in the range of the investigated concentrations The lowest detected concentration of toluene and ethanol were 0. 222 2 0μg/mL and 0. 197 3 0μg/mL,respectivcly. RSD of precision was 2. 2%0 and 2.0% （n =5）,respectively. The average recovery rates of toluene and ethanol were 101.8% and 100. 6% ,with RSD were 2. 2% and 1.2% （n =6）,respectively. Conlusion The established method is simple and sensitive with accurate and reliable detection results ,which could be used for the detection of residual solvents in haloperidol raw material drug.