油菜磷脂中溶剂残留检测

建立用气相色谱（GC）测定油菜磷脂中残留溶剂乙醇和丙酮的方法.采用玻璃毛细管色谱柱（30 m×250μm×0.25μm）,N₂为载气,FID检测器,正丙醇为溶剂,顶空进样,外标法计算残留溶剂的含量.顶空进样条件为平衡温度70℃;平衡时间45 min;溶剂体积比30%;进样量为10 mL.乙醇、丙酮、正丙醇、均完全分离;乙醇和丙酮在25～500μg/mL的范围内线性关系良好,R²分别为0.9997和0.9994;平均加样回收率乙醇为95.8%（n=5）,丙酮为98.5%（n=5）;检测限分别为乙醇17.0μg/mL,丙酮2.3μg/mL.实验方法方便简便、重复性好,结果准确.

Determination of residual ethanol and acetone in rapeseed phospholipid by GC

To develop a method for determining residual solvents such as ethanol and acetone in rapeseed phospholipid by gas chromatography(GC),the GC was equipped with a FID detector.A glass capillary column(30 m×250μm×0.25μm) was adopted with nitrogen as carrier gas and propanol as the solvent by headspace sampling.The assay of residual solvents were calculated according to the external standard method.Headspace sampling conditions were equilibrium temperature 70℃;equilibrium time 45 min;solvent volume ratio 30%;injection volume was 10 mL.Ethanol and acetone were detected as good separation.The standard curves were linear within the ranges of 25～500μg/mL for ethanol and acetone(R~2=0.999 7,0.999 4).The average recoveries were 95.8%(n=5)for ethanol,98.5%(n=5)for acetone.The limits of detection were 17.0μg/mL for ethanol,2.3μg/mL for acetone.This method appears to be sensitive accurate repeatable and easy to operate.