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目的建立气相色谱-质谱法(gas chromatography-mass spectrometry,GC-MS)测定鱼油中生育酚含量的分析方法。方法样品经正己烷提取,以HP-5MS毛细管柱分离,GC-MS选择离子检测模式测定。结果α-、γ-和δ-生育酚在0.002~0.04 mg/mL的浓度范围内呈良好线性关系,相关系数r2>0.999。此方法α-、γ-和δ-生育酚的检出限(S/N=3)分别为0.001、0.002、0.001 mg/g,定量限(S/N=10)为0.003、0.006、0.004 mg/g。在不同添加水平下,方法的平均回收率分别为98.6%~99.9%,相对标准偏差小于1.0%(n=3)。结论该方法简便、快速、灵敏、准确,适合鱼油中生育酚的定性和定量测定。
Objective To establish a method for the determination of tocopherols in fish oil by gas chromatography-mass spectrometry (GC-MS). Methods The samples were extracted with n-hexane, separated by HP-5MS capillary column and determined by GC-MS selective ion detection. Results The results showed that there was a good linear relationship between the concentrations of α-, γ- and δ-tocopherol in the range of 0.002-0.04 mg / mL with the correlation coefficient r2> 0.999. The detection limits (S / N = 3) of α-, γ- and δ-tocopherol were 0.001,0.002,0.001 mg / g and the limit of quantitation (S / N = 10) were 0.003,0.006,0.004 mg / g. The average recoveries of the methods were 98.6% ~ 99.9% and the relative standard deviations were less than 1.0% (n = 3) at different levels. Conclusion The method is simple, rapid, sensitive and accurate and suitable for qualitative and quantitative determination of tocopherols in fish oil.