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    超高效液相色谱法测定食品接触材料中间苯二甲酸和对苯二甲酸特定迁移量

    Determination of Specific Migration of m-phthalic Acid and p-phthalic Acid in Food Contact Materials by Ultra High Performance Liquid Chromatography

    • 摘要: 建立了超高效液相色谱法(UHPLC)测定食品接触材料聚对苯二甲酸乙二醇酯(PET)中的间苯二甲酸和对苯二甲酸特定迁移量的方法。按照以下参数进行迁移试验:①参考方法为国家标准GB 5009.156-2016和GB/T 23296.1-2009;②模拟液为4%(体积分数)乙酸溶液、10%(体积分数)乙醇溶液、20%(体积分数)乙醇溶液、50%(体积分数)乙醇溶液和橄榄油;③迁移温度为70℃,迁移时间为2 h。得到的迁移溶液供UHPLC进行分析,选择ShimSen-VD C30色谱柱为固定相,以体积比为40:60的甲醇和7.5 mmol·L-1磷酸二氢钾-磷酸缓冲溶液(pH 3.0)的混合溶液为流动相进行等度洗脱,在230 nm处用二极管阵列检测器(DAD)测定。以邻苯二甲酸为内标、用5种模拟液配制混合标准溶液系列,结果表明:对苯二甲酸、间苯二甲酸的线性范围为0.5~15.0 mg·L-1,检出限(3S/N)为0.03~0.07 mg·L-1。对实际样品进行3个浓度水平的加标回收试验,得到对苯二甲酸、间苯二甲酸的回收率为92.4%~106%,测定值的相对标准偏差(n=6)为0.17%~5.0%。用此方法分析了PET样品,未发现有这两种物质的迁移。

       

      Abstract: A method was developed for the simultaneous determination of migration amount of m-phthalic acid and p-phthalic acid in food contact material of ethylene terephthalate (PET) by ultra high performance liquid chromatography (UHPLC). Parameters for migration test were as follows:① national standards of GB 5009.156-2016 and GB/T 23296.1-2009 were adopted as reference methods; ② 4% (volume fraction) acetic acid solution, 10% (volume fraction) ethanol solution, 20% (volume fraction) ethanol solution, 50% (volume fraction) ethanol solution and olive oil were used as simulant solutions; ③ migration temperature was 70℃, and migration time was 2 h. The obtained migration solution was analyzed by UHPLC. ShimSen-VD C30 chromatographic column was selected as the stationary phase. The mixture of methanol and 7.5 mmol·L-1 potassium dihydrogen phosphate-phosphate buffer solution (pH 3.0) at volume ratio of 40:60 was used as the mobile phase for isocratic elution, and the content of p-phthalic acid and m-phthalic acid was determined with DAD at 230 nm. Using phthalate as the internal standard, a series of mixed standard solutions were prepared with above 5 simulant solutions. The results showed that linearity ranges of p-phthalic acid and m-phthalic acid was found within 0.5-15.0 mg·L-1, with detection limits (3S/N) in the range of 0.03-0.07 mg·L-1. The spiked recovery test was made on the actual sample at three concentration levels, giving results of p-phthalic acid and m-phthalic acid in the range of 92.4%-106%, and RSDs (n=6) of the determined values (n=6) ranged from 0.17% to 5.0%. The PET samples were analyzed by the proposed method, and no migration of these two substances was found.

       

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