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

作　　者：蔡翔宇 陈璐 吴玉杰 胡长鹰[3] 吕晓敏 CAI Xiang-Yu;CHEN Lu;WU Yu-Jie;HU Chang-Ying;LV Xiao-Min(Nanning Customs Technical Center,Nanning 530021,China;Chinese Academy of Inspection and Quarantine,Beijing 100176,China;Key Laboratory of Product Packaging and Logistics of Guangdong Higher Education Institutes,College of Packaging Engineering,Jinan University,Zhuhai 519070,China)

机构地区：[1]南宁海关技术中心,南宁530021 [2]中国检验检疫科学研究院,北京100176 [3]暨南大学包装工程学院,广东省普通高校产品包装与物流重点实验室,珠海519070

出　　处：《食品安全质量检测学报》2021年第15期5974-5982,共9页Journal of Food Safety and Quality

基　　金：国家重点研发计划项目(2018YFC1603205/2018YFC1603200)。

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2.5-100.0μg/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0.4-3.0μg/kg。在0.5-10.0 ng/mL和2.0-25.0μg/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。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.

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 

分 类 号：O657.63[理学—分析化学] TS201.6[理学—化学]