顶空气相色谱法测定叶黄素中有机溶剂残留量

Determination of residual organic solvents in lutein by headspace gas chromatography

目的 建立叶黄素中正己烷、乙醇和乙酸乙酯有机溶剂残留量的顶空气相色谱分析方法,并用该方法 测定样品中的有机溶剂残留量.方法采用顶空气相色谱法,色谱柱为DB-624毛细管色谱柱（30 m×0.53 mm×3 μm）,载气为氦气,检测器为氢火焰离子化检测器,以程序升温方式使正己烷、乙醇和乙酸乙酯达到完全分离,外标法定量.结果 正己烷、乙醇和乙酸乙酯的线性范围分别为4.95～198 mg/L （r=0.99998）、8.295～331.8 mg/L（r=0.99994）和8.325～333 mg/L（r=0.99999）;平均回收率范围为97.79％～103.21％,精密度（以相对标准偏差计,n=3）为1.47％～3.46％;检测限分别为0.09、0.83和0.33 mg/L.利用本方法对实际样品叶黄素中有机溶剂残留量进行了测定,结果表明,该样品中含有正己烷和乙醇,其含量分别为12 mg/kg和45 mg/kg.结论 本方法快速、灵敏、准确,适用于叶黄素中残留溶剂的检测.

Objective：A method for determination of three kinds of organic solvents residuals in lutein was developed by headspace gas chromatography,and the method was applied to analyze the organic solvents residuals in lutein samples.Methods：An DB-624 capillary column （30 m 0.53 mm 3 μm）,a flame ionization detector,helium and the external standard method were used for the separation and quantitative analysis.N-hexane,ethanol and ethyl acetate were separated completely using temperature program.Results：The standard curves showed linear property in the range of 4.95 ～198 mg/L （r=0.99998） for n-hexane,8.295 ～331.8 mg/L （r =0.99994） for ethanol and 8.325 ～333 mg/L （r =0.99999） for ethyl acetate.The recoveries for three residual organic solvents were between 97.79 ％ and 103.21％ with relative standard deviations （RSDs） （n =3） of 1.47 ％ ～ 3.46 ％.Limits of detection （LOD） of n -hexane,ethanol and ethyl acetate were 0.09,0.83 and 0.33 mg/L,respectively.The proposed method was successfully applied to determine the residual organic solvents in lutein sample.The results showed only n-hexane and ethanol were found in the sample with the contents of 12 mg/kg and 45 mg/kg,respectively.Conclusion：The method is rapid,sensitive and accurate for determination of solvents residuals in lutein.