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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。
A UPLC / Orbitrap HRMS method was developed for the rapid screening of photostabilizers and antioxidants in tetrahydrofuran-soluble plastic food contact materials And confirmed. The method comprises the following steps of: dissolving a plastic food contact material with tetrahydrofuran to obtain a clear solution; precipitating with methanol; centrifuging the solution; filtering the solution through a 0.22 μm filter for UPLC / Orbitrap HRMS analysis; Legal quantity. Chromatographic separation of 19 light stabilizers and 21 antioxidants was performed on a Hypersil GOLD column (100 mm × 2.1 mm × 1.9 μm) using a mobile phase of methanol / water with gradient elution. Mass spectrometry was carried out by first-order mass spectrometry in the range of 150-1 500 with electrospray positive and negative ions (ESI +, ESI-) mode respectively. The mass spectra were screened by retention time and quasi- The mass spectra accuracy of 19 light stabilizers and 21 antioxidants were all less than 2 × 10 -6. The limit of quantification was 0.01 ~ 1.00μg / kg. The average recoveries were 81.85% ~ 94.65% and the relative standard deviations (RSDs) were 3.25% ~ 9.99% at three different spiked levels. This method was used to screen commercially available plastic food contact materials. As a result, different levels of light stabilizers and antioxidants were detected in some samples.