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采用高效液相色谱–串联质谱(LC–MS/MS)技术建立了食品接触材料中20种邻苯二甲酸酯类迁移量的测定方法。样品分别采用欧盟(EU)No.10/2011法规中食品模拟液浸泡,橄榄油浸泡液用乙腈进行液–液萃取,水基浸泡液直接过滤,C18色谱柱(100 mm×2.1 mm,2.7μm)分离,以0.1%甲酸溶液–甲醇溶液为流动相,梯度洗脱,采用多反应监控(MRM)模式进行分析检测。20种邻苯二甲酸酯类化合物质量浓度在1~500 ng/m L范围内与色谱峰面积呈线性关系。水溶液、3%乙酸食品模拟浸泡液、10%乙醇食品模拟浸泡液、20%乙醇食品模拟浸泡液、50%乙醇食品模拟浸泡液、橄榄油食品模拟浸泡液中方法定量限分别为0.20~9.81 ng/m L,0.19~9.76 ng/m L,0.25~12.3ng/m L,0.21~10.8 ng/m L,0.19~11.7 ng/m L,0.45~20.3 ng/m L。样品加标回收率为85.8%~111.3%(3%乙酸浸泡液),79.4%~123.6%(橄榄油浸泡液),两种浸泡液中测定结果的相对标准偏差不大于8.48%(n=6)。该方法具有快速简便、灵敏度高及准确性好等特点,适用于塑料类食品接触材料中邻苯二甲酸酯类迁移量的检测。
A method for the determination of 20 kinds of phthalates migration in food contact materials was established by high performance liquid chromatography-tandem mass spectrometry (LC-MS / MS). The samples were respectively soaked in food simulants in EU Regulation No.10 / 2011. The olive oil soaking solution was subjected to liquid-liquid extraction with acetonitrile. The water-based soaking solution was directly filtered. The C18 column (100 mm × 2.1 mm, 2.7 μm ). The mobile phase was eluted with 0.1% formic acid in methanol. The gradient elution was carried out and analyzed by MRM (Multiple Reaction Monitoring). The concentration of 20 phthalates in the range of 1 ~ 500 ng / m L showed a linear relationship with the chromatographic peak area. The limit of quantification for the soaking solution in water, 3% acetic acid simulated soaking solution, 10% ethanol simulated soaking solution, 20% ethanol simulated soaking solution, 50% ethanol simulated soaking solution and olive oil food soaking solution were 0.20 ~ 9.81 ng / m L, 0.19 ~ 9.76 ng / m L, 0.25 ~ 12.3 ng / m L, 0.21 ~ 10.8 ng / m L, 0.19 ~ 11.7 ng / m L, 0.45 ~ 20.3 ng / m L. The recoveries of spiked samples ranged from 85.8% to 111.3% (3% acetic acid soaking solution) and from 79.4% to 123.6% (olive oil soaking solution). The relative standard deviations (RSDs) were not more than 8.48% ). The method has the characteristics of quick and easy, high sensitivity and good accuracy, and is suitable for the detection of the phthalate migration in plastic food contact materials.