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建立凝胶渗透色谱结合气相色谱-串联质谱(GC-MS/MS)同时测定食品中3种抗氧化剂的定性、定量分析方法。样品经正己烷饱和的乙腈提取,凝胶渗透色谱仪净化后,在30m长的气相毛细管色谱柱上分离,GC-MS/MS以多反应离子监测方式(SRM)检测目标化合物。结果表明:该方法在0.05～10mg/L范围内线性关系良好,相关系数(r)大于0.99。添加质量浓度为0.5～2.0mg/L时,抗氧化剂的回收率为77.6%～95.4%,相对标准偏差为2.7%～8.5%。方法的检出限(LOD)为0.03～0.10mg/kg(以3倍性噪比计)。本方法具有提取效率高,净化效果好,准确灵敏等优点,适用于食品中多种抗氧化剂的检测。
To establish a qualitative and quantitative method for the simultaneous determination of three antioxidants in foods by gel permeation chromatography coupled with gas chromatography-tandem mass spectrometry (GC-MS / MS). Samples were extracted with acetonitrile saturated with n-hexane, purified by gel permeation chromatography, and separated on a 30-m capillary gas chromatographic column. The target compounds were detected by multi-reactive ion monitoring (SRM) using GC-MS / MS. The results show that the method has a good linearity in the range of 0.05 ~ 10 mg / L and the correlation coefficient (r) is greater than 0.99. The recoveries of antioxidants ranged from 77.6% to 95.4% and the relative standard deviations (RSDs) ranged from 2.7% to 8.5% with the mass concentration of 0.5-2.0 mg / L. The limit of detection (LOD) of the method was 0.03 to 0.10 mg / kg (triploid to noise ratio). The method has the advantages of high extraction efficiency, good purification effect, accurate sensitivity and the like, and is suitable for the detection of multiple antioxidants in foods.