顶空-气相色谱法测定南极磷虾油中有机溶剂残留量

Determination of residual levels of organic solvents in Antarctic krill oil by headspace-gas chromatography

目的基于顶空-气相色谱法(headspace-gas chromatography,HS-GC),建立同时测定南极磷虾油中甲醇、丙酮、异丙醇、正己烷和乙酸乙酯5种有机溶剂残留的方法。方法样品溶解于苯甲醇,顶空进样器80℃平衡10 min,有机溶剂经DB-624毛细管色谱柱(60 m×0.32 mm,1.8μm)分离,氢火焰离子化检测器(flame ionization detector,FID)检测。对该方法进行了方法学验证,并实际应用于样品的分析测定。结果HS-GC可以将5种待测溶剂以及内标物很好地进行分离。标准曲线在所考察的浓度范围内线性良好,相关系数为0.9992~1.0000,检出限为0.6~9.0 mg/kg,定量限为1.2~15.0 mg/kg。方法日内精密度和日间精密度良好,在3个不同添加水平下,平均加标回收率为80.5%~105.0%,符合测定需求。结论该方法简单快捷,无需复杂前处理过程,结果可靠,可用于南极磷虾油中有机溶剂残留量的大规模快速检测。

Objective To establish a method for the determination of 5 kinds of residual organic solvents,including methanol,acetone,isopropanol,hexane and ethyl acetate,in Antarctic krill oil simultaneously by headspace-gas chromatography(HS-GC).Methods The samples were solved in the benzyl alcohol and equilibrated in the headspace at 80℃for 10 min.After being separated with DB-624 capillary column(60 m×0.32 mm,1.8μm),the organic solvents were detected by flame ionization detector(FID).The method was verified and applied for sample analysis.Results All 5 kinds of residual solvents could be separated from the internal standard completely.Within the investigated concentration scope,the standard curves were linear and the correlation coefficients were 0.9992‒1.0000.The limits of detection were 0.6‒9.0 mg/kg and the limits of quantitative were 1.2‒15.0 mg/kg,with excellent intra-day and inter-day precisions.The mean recoveries ranged from 80.5%to 105.0%at 3 spiking levels,which met the determination requirements.Conclusion As a simple,rapid and reliable method without complex pretreatment process,it can be used for large-scale and rapid detection of organic solvents in Antarctic krill oil.