顶空气相色谱法测定弹性酶中有机溶剂残留量

目的建立弹性酶原料中4种有机溶剂残留量的测定方法。方法采用顶空气相色谱法,FID检测器,分别在系统一:FFAP毛细管柱(30 m×0.32 mm,1.8μm),程序升温(80℃保持15 min,以30℃/min升至220℃,保持5 min);系统二:DB-624毛细管柱(30 m×0.32 mm,1.8μm),程序升温(40℃保持8 min,以30℃/min升至220℃,保持5 min);顶空条件均为85℃平衡30 min,进样口温度均为250℃,检测器温度均为250℃,载气为氮气,以水为溶剂配制对照品溶液及样品溶液,采用外标法定量。结果 4种残留溶剂在对应于限度的50%～150%浓度范围内有良好的线性关系(r=0.996 6～0.999 5),平均回收率为92.1%～103.3%。结论该法简便快捷,能准确有效地控制产品的质量。

Determination of residual organic solvents in elastase by headspace gas chromatography

Purpose To establish the methods for determination of four kinds of residual organic solvents in elastase.Methods Capillary column was used with temperature program and FID detector by headspace at injection temperature of 85 ℃ and equilibrium 30 min,using nitrogen as the carrying gas.The first system:FFAP capillary column(30 m×0.32 mm,1.8 μm).The column temperature was initially maintained at 80 ℃ for 15 min,then increased to 220 ℃ at the rate of 30 ℃ per min and maintained for 5 min.The second system:DB-624 capillary column(30 m×0.32 mm,1.8 μm).The column temperature was initially maintained at 40 ℃ for 8 min,then increased to 220 ℃ at the rate of 30 ℃ per min and maintained for 5 min.The injector temperature was maintained at 250 ℃ and the detector temperature was 250 ℃.Results The recoveries were 92.1%-103.3% and excellent linearity was obtained(r=0.996 6-0.999 5) between the corresponding concentrations of 50% limits and 150% limits.Conclusion The method was sensitive,accurate,rapid and suitable for quality control.