顶空毛细管气相色谱法测定维生素A棕榈酸酯中5种有机溶剂残留量

Capillary GC Determination of 5 Residual Organic Solvents in Vitamin A Palmitate with Headspace Sampling

目的建立维生素A棕榈酸酯中残留溶剂的测定法。方法采用气相色谱法:用固定相为100%聚乙二醇(ZB-WAX)的毛细管柱,载气为氮气,火焰离子化检测器(FID),进样口温度为200℃,检测器温度为250℃,柱温采用程序升温,初始温度50℃,保持3min,再以60℃/min的升温速度升至120℃,保持5 min。柱流速为1.34 mL/min,顶空温度为80℃,顶空平衡时间为30 min,顶空进样体积为1.0 mL。结果各残留溶剂溶液浓度均与峰面积线性关系良好,平均回收率为97.6%～107.5%,方法准确度良好。结论本方法操作简便,结果可靠,重复性好,可以用于维生素A棕榈酸酯中残留溶剂的检测。

Objective To establish a method for the determination of residual organic solvents in Vitamin A palmitate.Methods The residual organic solvents were determined by GC with capillary column（ZB-WAX） with FID detector and headspace sampling,nitrogen as the carrier gas.The temperature of the injection port was maintained at 200 ℃ and that of detector at 250 ℃.The initial column temperature was 50 ℃,maintained for 3 min,then raised to 120 ℃ at a rate of 60 ℃/min,and maintained for 5 min.The column flow was 1.34 mL/min,headspace oven was set at a temperature of 80 ℃ for 30 min and the injection volume was 1 mL with headspace sampling.Results The calibration curves of residual organic solvents was in a good linearity,the recoveries of residual organic solvents were between 97.6% and 107.5%,with good accuracy.Conclusion The method is simple and reliable,with good repeatability.It is applicable for the quality control of residual organic solvents in vitamin A palmitate.