塑料食品接触材料中光稳定剂和抗氧剂的快速筛查和确证

Rapid Screening and Confirmation of Light Stabilizers and Antioxidants in Plastic Materials Intended to Come into Contact with Foodstuffs

建立了一种超高效液相色谱/静电场轨道阱高分辨质谱(UPLC/Orbitrap HRMS)联用法,对可溶于四氢呋喃的塑料食品接触材料中的光稳定剂和抗氧剂进行了快速筛查和确证。该方法首先用四氢呋喃溶解塑料食品接触材料,得到澄清溶液,再用甲醇进行沉淀,并离心分离,所得溶液经0.22μm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。19种光稳定剂和21种抗氧剂的色谱分离在Hypersil GOLD色谱柱(100 mm×2.1 mm×1.9μm)上完成,流动相为甲醇/水,洗脱方式为梯度洗脱。质谱分析分别采用电喷雾正负离子(ESI+、ESI-)模式,在m/z为150~1 500范围内进行一级质谱全扫描,利用保留时间和准分子离子精确质量数进行筛查,利用二级质谱图进行确证,19种光稳定剂和21种抗氧剂的质量数精确度误差均小于2×10^(-6)。方法的定量限为0.01~1.00μg/kg。在3个不同加标浓度水平下,方法的平均加标回收率为81.85%~94.65%,相对标准偏差为3.25%~9.99%。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含量水平的光稳定剂和抗氧剂。

An effective method was established for the rapid screening and confirmation of light stabilizers and antioxidants in plastic materials intended to come into contact with foodstuffs,which could be dissolved in tetrahydrofuran,using ultra-high performance liquid chromatography/orbitrap high resolution mass spectrometry（UPLC/Orbitrap HRMS） technique.Plastic materials intended to come into contact with foodstuffs were first dissolved completely by tetrahydrofuran to obtain a transparent solution,then the transparent solution was precipitated with methanol,followed by centrifugal separation.The proposed solution was filtered by 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 nineteen light stabilizers and twenty one antioxidants were carried out on an Hypersil GOLD column（100 mm×2.1 mm,1.9 μm） with a gradient elution of methanol/water.The mass spectrometric analysis was carried out by Orbitrap HRMS in ESI＋ and ESI-mode,respectively.Full-scan experiment was carried out in the range of m/z 150 to m/z 1 500.The screening and qualitative analysis were carried out by the retention time and the exact mass of quasi-molecular ion.The confirmation analysis for target compounds was performed with the daughter ions in dd MS2 mode.Nineteen light stabilizers and twenty one antioxidants were routinely detected with the mass accuracy below 2×10^（-6）.The limits of quantification（LOQ） 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 81.85% to 94.65% while the relative standard deviation（RSD） varied from 3.25% to 9.99%.The proposed method was applied in the rapid screening of light stabilizers and antioxidants in plastic materials intended to come into contact with foodstuffs available commercially.Some light stabilizers and antioxidants at different content levels were detected in some samples.