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采用液相色谱-高分辨质谱法对炊具中迁移性物质进行全面筛选,并对初级芳香胺进行目标分析。

Target analysis of primary aromatic amines combined with a comprehensive screening of migrating substances in kitchen utensils by liquid chromatography-high resolution mass spectrometry.

机构信息

Foundation for the Promotion of the Health and Biomedical Research in the Valencia Region (FISABIO-Public Health), 21, Avenida Catalunya, 46020 Valencia, Spain; Public Health Laboratory of Valencia, 21, Avenida Catalunya, 46020 Valencia, Spain.

Foundation for the Promotion of the Health and Biomedical Research in the Valencia Region (FISABIO-Public Health), 21, Avenida Catalunya, 46020 Valencia, Spain; Public Health Laboratory of Valencia, 21, Avenida Catalunya, 46020 Valencia, Spain; Analytical Chemistry Department, University of Valencia, Edifici Jeroni Muñoz, Dr. Moliner 50, 46100 Burjassot, Spain.

出版信息

Talanta. 2015 Jun 1;138:290-297. doi: 10.1016/j.talanta.2015.03.026. Epub 2015 Mar 23.

Abstract

An analytical strategy including both the quantitative target analysis of 8 regulated primary aromatic amines (PAAs), as well as a comprehensive post-run target screening of 77 migrating substances, was developed for nylon utensils, using liquid chromatography-orbitrap-high resolution mass spectrometry (LC-HRMS) operating in full scan mode. The accurate mass data were acquired with a resolving power of 50,000 FWHM (scan speed, 2 Hz), and by alternating two acquisition events, ESI+ with and without fragmentation. The target method was validated after statistical optimization of the main ionization and fragmentation parameters. The quantitative method presented appropriate performance to be used in official monitoring with recoveries ranging from 78% to 112%, precision in terms of Relative Standard Deviation (RSD) was less than 15%, and the limits of quantification were between 2 and 2.5 µg kg(-1). For post-target screening, a customized theoretical database was built for food contact material migrants, including bisphenols, phthalates, and other amines. For identification purposes, accurate exact mass (<5 ppm) and some diagnostic ions including fragments were used. The strategy was applied to 10 real samples collected from different retailers in the Valencian Region (Spain) during 2014. Six out of eight target PAAs were detected in at least one sample in the target analysis. The most frequently detected compounds were 4,4'-methylenedianiline and aniline, with concentrations ranging from 2.4 to 19,715 µg kg(-1) and 2.5 to 283 µg kg(-1), respectively. Two phthalates were identified and confirmed in the post-run target screening analysis.

摘要

开发了一种分析策略,用于分析尼龙器具中的 8 种受管制的芳香胺(PAA),并在运行后对 77 种迁移物质进行全面的目标筛查,该策略采用液相色谱-轨道阱-高分辨率质谱(LC-HRMS),以全扫描模式运行。精确质量数据是在分辨率为 50,000 FWHM(扫描速度为 2 Hz)的条件下,通过交替进行两种采集事件,即带和不带碎片的 ESI+采集事件获得的。该目标方法在对主要离子化和碎裂参数进行统计优化后进行了验证。该定量方法表现出适当的性能,可用于官方监测,回收率范围为 78%至 112%,相对标准偏差(RSD)的精密度小于 15%,定量限在 2 至 2.5 µg kg(-1)之间。对于目标后筛查,为食品接触材料迁移物建立了定制的理论数据库,其中包括双酚、邻苯二甲酸酯和其他胺类。为了进行鉴定,使用了精确的精确质量(<5 ppm)和一些包括碎片在内的诊断离子。该策略应用于 2014 年在瓦伦西亚地区(西班牙)的不同零售商收集的 10 个实际样品。在目标分析中,至少有一个样品检测到了 8 种目标 PAA 中的 6 种。检测到的最常见化合物是 4,4'-亚甲基二苯胺和苯胺,浓度范围分别为 2.4 至 19,715 µg kg(-1)和 2.5 至 283 µg kg(-1)。在后运行目标筛查分析中,鉴定并确认了两种邻苯二甲酸酯。

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