顶空气相色谱法测定弹性酶中有机溶剂残留量

Determination of residual organic solvents in elastase by headspace gas chromatography

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。

Purpose To establish the methods for determination of four kinds of residual organic sol- vents in elastase. Methods Capillary column was used with temperature program and FID detector by headspace at injection temperature of 85 ~C and equilibrium 30 rain,using nitrogen as the carrying gas. The first system ： FFAP capillary column （30 m × 0.32 mm, 1.8 μm）. The column temperature was ini- tially maintained at 80 ~C for 15 min,then increased to 220℃ at the rate of 30 ℃ per rain and main- tained for 5 rain. The second system ： DB-624 capillary column （30 m x 0.32 ram, 1.8 μm）. The column temperature was initially maintained at 40 ℃ for 8 rain,then increased to 220 ℃at the rate of 30 ℃ per rain and maintained for 5 rain. The injector temperature was maintained at 250 ℃and the detector tem- perature was 250 ℃. Results The recoveries were 92. 1%-103.3% and excellent linearity was obtained （r = 0. 996 6-0. 9995） between the corresponding concentrations of 50% limits and 150% limits. Con- clusion The method was sensitive, accurate, rapid and suitable for quality control.