高效液相色谱-串联质谱法同时测定聚对苯二甲酸乙二醇酯/聚乙烯复合食品接触材料中16种抗氧化剂特定迁移量

Simultaneous determination of specific migration limits of 16 kinds of antioxidants in food contact polyethylene glycol terephthalate/ polyethylene composite materials by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法  抗氧化剂  特定迁移量  聚对苯二甲酸乙二醇酯/聚乙烯

英文关键词:high performance liquid chromatography-tandem mass spectrometry  antioxidants  specific migration limit  polyethylene glycol terephthalate/polyethylene

中文摘要:

      目的 建立高效液相色谱-串联质谱法同时测定16种抗氧化剂从聚对苯二甲酸乙二醇酯/聚乙烯(polyethylene glycol terephthalate/polyethylene, PET/PE)复合食品接触材料中迁移至超纯水、3% (V/V)乙酸、10%乙醇和橄榄油这4种食品模拟物的特定迁移量的方法。方法 考察不同实验条件对橄榄油食品模拟物中16种抗氧化剂的提取效果。采用ODS色谱柱梯度洗脱分离, 以甲醇和水作为流动相梯度洗脱, 在正、负离子模式下以电喷雾电离多反应监测模式(multiple reaction monitoring, MRM)进行测定, 外标法定量。结果 16种目标化合物在0.5~20.0 ng/mL及2.5~100.0 μg/kg范围内具有良好的线性关系, 相关系数均大于0.998, 水性食品模拟物(超纯水、3%乙酸、10%乙醇)的定量限为0.1~1.3 ng/mL, 橄榄油食品模拟物的定量限为0.4~3.0 μg/kg。在0.5~10.0 ng/mL和2.0~25.0 μg/kg加标水平下的平均回收率为81.0%~112.5%, 相对标准偏差为0.4%~9.1%。结论 该方法灵敏度高、定量限低, 满足PET/PE复合食品接触材料中抗氧化剂特定迁移量的检测要求。

英文摘要:

      Objective To establish a method for simultaneous determination of the specific migration of 16 kinds of antioxidants from polyethylene glycol terephthalate/polyethylene (PET/PE) to 4 kinds of food simulants of ultrapure water, 3% (V/V) acetic acid, 10% (V/V) ethanol, olive oil by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The extraction effects of 16 kinds of antioxidants from olive oil food simulators were investigated under different experimental conditions. The analytes were separated with ODS chromatographic column using methanol/water as mobile phase for gradient elution. Finally, the eluents were determined with multiple reaction monitoring (MRM) of electrospray ionization in positive/negative mode, quantified by the external standard method. Results The proposed method showed good linearities in the range of 0.5-20.0 ng/mL and 2.5-100.0 μg/kg with the correlation coefficients above 0.998 for all 16 kinds of target compounds. The limits of quantification of water-based food simulators (ultra-pure water, 3% acetic acid, 10% ethanol) were 0.1?1.3 ng/mL, and the limits of quantification of olive oil food simulators were 0.4?3.0 μg/kg. The recoveries at spiked concentration levels of 0.5?10.0 ng/mL and 2.0?25.0 μg/kg were between 81.0% and 112.5% with relative standard deviations of 0.4%?9.1%. Conclusion The method has high sensitivity and low limit of quantification, and can meet the requirements of the specific migration limits of antioxidants in food contact PET/PE composite materials.