Moreta Cristina, Tena María-Teresa
Department of Chemistry, University of La Rioja, C/Madre de Dios 51, E-26006, Logroño (La Rioja), Spain.
J Chromatogr A. 2015 Oct 2;1414:77-87. doi: 10.1016/j.chroma.2015.08.030. Epub 2015 Aug 18.
A simple and sensitive analytical method for the determination of several plastic additives in multilayer packaging based on solid-liquid extraction (SLE) and ultra-high performance liquid chromatography (UHPLC) coupled to variable wavelength (VWD) and time of flight mass spectrometry (TOF-MS) detectors is presented. The proposed method allows the simultaneous determination of fourteen additives belonging to different families such as antioxidants, slip agents and light stabilizers, as well as two oxidation products in only 9min. The developed method was validated in terms of linearity, matrix effect error, detection and quantification limits, repeatability and intermediate precision. The instrumental method showed satisfactory repeatability and intermediate precision at concentrations closed to LOQ with RSDs less than 7 and 20%, respectively, and LODs until 5000 times more sensitive than other GC-FID and HPLC-VWD methods previously reported. Also, focused ultrasound solid-liquid extraction (FUSLE) was optimized and evaluated to extract plastic additives from packaging. Extraction results obtained by FUSLE and SLE were compared to those obtained by pressurized liquid extraction (PLE). All extraction methods showed excellent extraction efficiency for slip agents, however quantitative recovery of all analytes was achieved only by SLE with just 5ml of hexane for 10h. Finally, the selected method was applied to the analysis of packaging samples where erucamide, Irgafos 168, oxidized Irgafos 168, Irganox 1076 and Irganox 1010 were detected and quantified.
本文提出了一种基于固液萃取（SLE）和超高效液相色谱（UHPLC）联用可变波长（VWD）和飞行时间质谱（TOF-MS）检测器的简单灵敏分析方法，用于测定多层包装中的几种塑料添加剂。该方法能够在仅9分钟内同时测定十四种属于不同类别的添加剂，如抗氧化剂、爽滑剂和光稳定剂，以及两种氧化产物。所开发的方法在线性、基质效应误差、检测限和定量限、重复性和中间精密度方面进行了验证。该仪器方法在接近定量限的浓度下显示出令人满意的重复性和中间精密度，相对标准偏差分别小于7%和20%，检测限比先前报道的其他气相色谱-火焰离子化检测器（GC-FID）和高效液相色谱-可变波长检测器（HPLC-VWD）方法灵敏高达5000倍。此外，还对聚焦超声固液萃取（FUSLE）进行了优化和评估，以从包装中提取塑料添加剂。将FUSLE和SLE获得的萃取结果与加压液体萃取（PLE）获得的结果进行了比较。所有萃取方法对爽滑剂均显示出优异的萃取效率，然而仅通过SLE使用5毫升己烷萃取10小时才能实现所有分析物的定量回收。最后，将所选方法应用于包装样品分析，检测并定量了芥酸酰胺、Irgafos 168、氧化Irgafos 168、Irganox 1076和Irganox 1010。
