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    顶空-气相色谱法测定聚乙烯食品接触材料中1-己烯、1-辛烯和乙酸乙烯酯在食品模拟物中的迁移量

    Headspace-GC Determination of Amounts of 1-Hexene, 1-Octene and Vinyl Acetate Migrated from Polyethylene Food-Contacting Materials into Food Simulants

    • 摘要: 试验中选择的食品模拟物为4种水基食品模拟物(体积分数为4%的乙酸溶液和体积分数为10%,20%,50%的乙醇溶液)和1种油基模拟物(橄榄油)。经迁移试验得到上述5种介质的食品模拟液。取4种水基食品模拟液各1.00 mL和油基食品模拟液1.000 g,分别置于5个顶空瓶中,各加入N,N-二甲基酰胺(DMF)200 μL,加盖密封。顶空平衡温度为80℃(水基食品模拟液)和100℃(油基食品模拟液),顶空平衡时间均为15 min。处于气态的组分(1-己烯、1-辛烯和乙酸乙烯酯)随即引入DB-WAX色谱柱(60 m×0.25 mm,0.25 μm)进行分离。上述3种被测物的保留时间依次为5.303,6.632,7.402 min。在上述5种食品模拟液中,3种被测物(1-己烯、1-辛烯和乙酸乙烯酯)的线性范围分别为0.5~5.0 mg·kg-1,2.5~25.0 mg·kg-1和2.0~20.0 mg·kg-1,其检出限(3S/N)为:1-己烯0.05 mg·kg-1(水基食品模拟物),0.2 mg·kg-1(油基食品模拟物);1-辛烯0.05 mg·kg-1(水基食品模拟物),1.0 mg·kg-1(油基食品模拟物);乙酸乙烯酯0.5 mg·kg-1(体积分数为50%乙醇溶液),0.2 mg·kg-1(其余3种水基食品模拟物)和1.0 mg·kg-1(油基食品模拟物)。在3个浓度水平上进行加标回收试验,测得回收率为88.0%~103%,测定值的相对标准偏差(n=5)为1.2%~7.9%。对20种聚乙烯食品接触材料样品进行分析,均未检出上述3种化合物。

       

      Abstract: Four water-based food simulants, i.e. 4% (φ) acetic acid solution, 10% (φ, the same below), 20% and 50% ethanol solutions, and one oil-based food simulant (olive oil) were selected as the food simulants. At the end of migration test, the food simulated solutions of the above 5 simulants were obtained, 1.00 mL aliquots were taken from the 4 water-based food simulated solutions and placed separately into 4 headspace flasks, and 1.000 g of the oil-based food simulated solution was taken and placed into the 5th headspace flask. 200 μL of DMF were added to each of the 5 headspace flasks, and after tight capping, the solutions were equilibrated separately with headspace for 15 min at 80℃ (for water-based food simulated solutions) and at 100℃ (for oil-based food simulated solution). The 3 analytes (1-hexene, 1-octene and vinyl acetate) in their gaseous state were introduced into the DB-WAX chromatographic column (60 m×0.25 mm, 0.25 μm) and separated according to their retention times of 5.303, 6.632, 7.402 min respectively. Linearity ranges of the 3 analytes in the above 5 food simulated solutions were found same between 0.5-5.0 mg·kg-1 for 1-hexene, between 2.5-25.0 mg·kg-1 for 1-octene and between 2.0-20.0 mg·kg-1 for vinyl acetate. Their detection limits (3S/N) found were:(for 1-hexene) 0.05 mg·kg-1 (in water-based food simulants), and 0.2 mg·kg-1 (in oil-based food simulant); (for 1-octene) 0.05 mg·kg-1 (in water-based food simulants), and 1.0 mg·kg-1 (in oil-based food simulant); (for vinyl acetate) 0.5 mg·kg-1 (in 50% ethanol solution), 0.2 mg·kg-1 (in the remainder 3 water-based food simulants), and 1.0 mg·kg-1 (in oil-based food simulant). Recovery was tested by standard addition at 3 concentration levels, giving results of recovery in the range of 88.0%-103% with values of RSDs (n=5) of determined values in the range of 1.2%-7.9%. Twenty samples of polyethylene food-contacting materials were analyzed by the method. Neither of the 3 analytes was found.

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