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    气相色谱-质谱法快速测定食品接触用塑料中2,2,4-三甲基-1,3-戊二醇双异丁酸酯的特定迁移量

    Rapid Determination of Specific Migration Amount of 2,2,4-Trimethyl-1,3-Pentanediol Diisobutyrate in Plastics for Food Contact by GC-MS

    • 摘要: 采用气相色谱-质谱法快速测定从食品接触用塑料中迁移至水、4%(体积分数,下同)乙酸溶液、20%(体积分数,下同)乙醇溶液、50%乙醇溶液、异辛烷和橄榄油等6种食品模拟物中2,2,4-三甲基-1,3-戊二醇双异丁酸酯的含量。在气相色谱分离中采用DB-5MS色谱柱(30 m×0.25 mm,0.25 μm),在质谱分析中采用选择离子监测模式。食品模拟物为水、4%乙酸溶液、20%乙醇溶液和50%乙醇溶液时,萃取溶剂为正己烷,萃取次数为1,萃取时间为10 min;食品模拟物为异辛烷时无需萃取;食品模拟物为橄榄油时,萃取溶剂为甲醇,萃取次数为3,萃取时间为10 min。TXIB的质量浓度在0.03~1.00 mg·L-1(食品模拟物为橄榄油:0.10~2.00 mg·kg-1)内与其对应的峰面积呈线性关系,检出限(3S/N)为0.01 mg·kg-1(食品模拟物为橄榄油:0.03 mg·kg-1),测定下限(10S/N)为0.03 mg·kg-1(食品模拟物为橄榄油:0.10 mg·kg-1)。以空白食品模拟物为基体进行加标回收试验,所得回收率为82.7%~110%,测定值的相对标准偏差(n=6)为2.3%~10%。

       

      Abstract: GC-MS was applied to the rapid determination of amount of 2,2,4-trimethyl-1,3-pentanediol diisobutyrate migrated from plastics for food contact into 6 food simulant, i.e.water, 4% (volume fraction, the same below) acetic acid solution, 20% (volume fraction, the same below) ethanol solution, 50% ethanol solution, isooctane and olive oil. The DB-5MS chromatographic column (30 m×0.25 mm, 0.25 μm) was used for GC separation and the selected ion monitoring mode was adopted in MS determination. When food simulants were water, 4% acetic acid solution, 20% ethanol solution and 50% ethanol solution, extraction solvent was n-hexane, extraction repeat was 1 and extraction time was 10 min; when food simulant was isooctane, no extraction was required; when food simulant was olive oil, extraction solvent was methanol, extraction repeat was 3 and extraction time was 10 min. Linear relationship between values of peak area and mass concentration of TXIB was kept in the range of 0.03-1.00 mg·L-1 (0.10-2.00 mg·kg-1 when food simulant was olive oil), with detection limit (3S/N) of 0.01 mg·kg-1 (0.03 mg·kg-1 when food simulant was olive oil) and lower limit of determination (10S/N) of 0.03 mg·kg-1 (0.10 mg·kg-1 when food simulant was olive oil). On the base of blank food simulants, test for recovery was made by standard addition method; values of recovery found were in the range of 82.7%-110%, with RSDs (n=6) of determined values in the range of 2.3%-10%.

       

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