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提出了固相萃取-气相色谱-质谱法测定辐照鱼油中2-烷基环丁酮(2-十二烷基环丁酮和2-十四烷基环丁酮)含量的方法。0.300g辐照鱼油样品用正己烷溶解,ProElut Silica固相萃取柱净化。在气相色谱分离中用HP-5MS色谱柱为固定相,在质谱分析中采用选择离子监测模式。2种2-烷基环丁酮的质量浓度均在0.01~1.0mg·L-1范围内与其峰面积呈线性关系,方法的测定下限(10S/N)为10μg·kg-1。加标回收率在91.2%~96.0%之间,测定值的相对标准偏差(n=6)在3.7%~5.9%之间。
A method for the determination of 2-alkylcyclobutanone (2-dodecylcyclobutanone and 2-tetradecylcyclobutanone) in irradiated fish oil by solid-phase extraction and gas chromatography-mass spectrometry was proposed. Samples of 0.300 g irradiated fish oil were dissolved in n-hexane and purified using a ProElut Silica cartridge. HP-5MS columns are used as the stationary phase in gas chromatographic separations and selective ion monitoring modes are used in mass spectrometry. The mass concentration of 2 kinds of 2-alkylcyclobutanone showed a linear relationship with the peak area in the range of 0.01-1.0 mg · L-1. The lower limit of determination (10S / N) was 10 μg · kg-1. The spiked recoveries ranged from 91.2% to 96.0%. The relative standard deviations (n = 6) were between 3.7% and 5.9%.