气相色谱-质谱联用法测定食品包装材料中4种苯酚类抗氧剂迁移量

Determination on Migration Quantity of Four Phenolic Antioxidants in Food Packaging Materials by Gas Chromatography-Mass Spectrometry

建立了气相色谱-质谱联用(GC-MS)测定食品包装材料中2,6-二甲基苯酚、对叔丁基苯酚、2,6-二叔丁基对甲酚和叔丁基-4-羟基苯甲醚迁移量的方法。采用水、4%(体积分数)乙酸、50%(体积分数)乙醇和异辛烷作为食品模拟物,样品经食品模拟物浸泡:水基模拟物浸泡液经乙酸乙酯液液萃取后测定,异辛烷浸泡液则直接测定。采用DB-1701色谱柱(30 m×0.25 mm×0.25μm)进行分离,选择离子模式进行检测,外标法定量。结果表明,在优化实验条件下,4种苯酚类抗氧剂在0.1~10 mg/L质量浓度范围内线性良好,相关系数(r)均大于0.999,方法检出限(LOD)均为0.01 mg/L,定量下限(LOQ)均为0.03 mg/L。在0.1、1.0、10.0 mg/L 3个加标水平下,方法的回收率为91.5%~110%,相对标准偏差(RSD,n=5)为1.9%~9.3%。该法准确、可靠、灵敏度高,适用于食品包装材料中4种苯酚类抗氧剂迁移量的测定。

A gas chromatography-mass spectrometric（GC-MS） method was established for the determination of migration quantity of 2,6-dimethylphenol,p-tert-butylphenol,2,6-di-tert-butyl-4-methylphenol and butylated hydroxyanisole in food packaging materials, with water, 4%（by volume） aqueous acetic acid,50%（by volume） aqueous ethanol and isooctane as the food simulated solution. Samples were soaked with food stimulant,and the water based food simulated soaking solution was extracted with ethyl acetate before analysis,while the isooctane soaking solution was analyzed without any pretreatment. The separation of target compounds was conducted using a DB-1701 capillary（30 m × 0. 25 mm × 0. 25 μm） column. The determination was performed in selective ion mode,and external standard method was used for quantitation. The results showed that,under optimized conditions,there were good linearities for four phenolic antioxidants between peak areas and concentrations in the range of 0. 1-10 mg/L with correlation coefficients（r） more than 0. 999. The limits of detection（LOD） of this method were 0. 01 mg/L,and the limits of quantitation（LOQ） were0. 03 mg/L. The spiked recoveries for four phenolic antioxidants in fruits at three spiked levels of0. 1,1. 0,10. 0 mg/L ranged from 91. 5% to 110%,with relative standard deviations（RSDs,n =5） of 1. 9%-9. 3%. The method,with the advantages of accuracy,high reliability and sensitivity,was suitable for the determination of migration of four phenolic antioxidants in food packaging materials.