超高效液相色谱/静电场轨道阱高分辨质谱法快速筛查塑料食品接触材料中抗氧剂

摘要

An effective method was established for rapid screening of 21 antioxidants in plastic materials be used for contact with foodstuffs using ultra-high performance liquid chromatography/orbitrap high resolution mass spectrometry (UPLC/Orbitrap HRMS)technique.Plastic materials be used for contact with foodstuffs were first dissolved completely with tetrahydrofuran to obtain a transparent solution,then this one was precipitated by methanol,followed by centrifugal separation.The proposed solution was filtered with 0.22 μm membrane,followed by the analysis of UPLC/Orbitrap HRMS.Quantitative analysis was carried out by the peak area in extracted chromatography and the external standard method was used in the quantitative analysis.The chromatographic separation of 21 antioxidants was carried out on an Hypersil GOLD column (100 mm (2.1 mm,1.9 μm) with a gradient elution of methanol/water.The mass spectrometry analysis was carried out by Orbitrap HRMS in ESI-mode.Full-scan experiment was carried out in the range of m/z 150 to m/z 1500.The screening and qualitative analysis were carried out by the retention time and the exact mass of the quasi-molecular ion and 21antioxidants were detected with mass accuracy error below 2 × 10-6 (2 ppm).The limits of quantification varied from 0.01 μg/kg to 1.00 μg/kg.The blank samples were spiked at three different levels and the average spiked recoveries changed from 81.74％ to 94.48％ while the relative standard deviation (RSD) changed from 2.95％ to 9.98％.The proposed method was applied in the rapid screening of antioxidants in commercially available plastic materials using for contact with foodstuffs and Irganox 1010 at different content levels were detected in some samples.%建立了一个超高效液相色谱/静电场轨道阱高分辨质谱(UPLC/Orbitrap HRMS)方法,对塑料食品接触材料中21种抗氧剂进行了快速筛查,该方法首先用四氢呋喃溶解塑料食品接触材料,所得溶液用甲醇沉淀,离心分离后,清液经0.22 μm滤膜过滤后进行UPLC/Orbitrap HRMS分析,利用提取离子色谱峰面积进行外标法定量.21种抗氧剂的色谱分离在Hypersil GOLD色谱柱(100 mm×2.1 mm,1.9 μm)上完成,流动相为甲醇/水,采取梯度洗脱方式.质谱分析采用电喷雾负离子(ESI)模式,在m/z 150～ m/z 1500范围内进行一级质谱全扫描.利用保留时间和准分子离子的精确质量数进行定性,21种抗氧剂的质量数精确度误差均小于2 ×10-6(2 pmm).21种抗氧剂的定量限为0.01～1.00 μg/kg,在3个不同加标浓度水平下,方法的平均加标回收率为81.74％ ～ 94.48％,相对标准偏差为2.95％～9.98％.应用本方法对市售塑料食品接触材料进行筛查,结果在部分样品中检出不同浓度水平的抗氧剂1010.