Food Characterization and Quality Department, Instituto de la Grasa, CSIC, Av Padre García Tejero 4, 41012 Seville, Spain.
Talanta. 2010 Mar 15;80(5):2076-82. doi: 10.1016/j.talanta.2009.11.008. Epub 2009 Nov 12.
A solvent-free analytical approach based on headspace solid-phase microextraction (SPME) of oil matrices heated at high temperatures coupled to gas chromatography with mass spectrometry detector (GC-ion trap) has been developed for the determination of phthalic acid esters (PAEs) in oil matrices without sample manipulation. For this study, three fibers, i.e., 85 microm-polyacrylate (PA), 50/30 microm-divinylbenzene-carboxen-polydimethylsiloxane (DVB/CAR/PDMS) and 100 microm-polydimethylsiloxane (PDMS) were tested. Variables affecting the SPME headspace composition such as incubation sample temperature, sample incubation time and fiber exposition time were optimized. The optimal values found were 250 degrees C for sample incubation temperature and 30 min for incubation and extraction time. PA fiber was not suitable for the lightest polar phthalates which showed poor extraction and repeatability values. PDMS fiber had very poor response for some of the heavier and non-polar phthalates, whereas DVB/CAR/PDMS fiber showed the best response and repeatability values for the majority of the phthalates studied. The main benefit of the analytical method proposed is the absence of sample manipulation and hence avoidance of possible contamination coming from glassware, environment, solvents and samples.
一种无溶剂分析方法，基于高温加热油基质中的顶空固相微萃取（SPME），与气相色谱-质谱检测器（GC-离子阱）联用，无需样品处理即可测定油基质中的邻苯二甲酸酯（PAE）。在这项研究中，测试了三种纤维，即 85 微米-聚丙烯酸酯（PA）、50/30 微米-二乙烯基苯-羧基-聚二甲基硅氧烷（DVB/CAR/PDMS）和 100 微米-聚二甲基硅氧烷（PDMS）。优化了影响 SPME 顶空成分的变量，如样品孵育温度、样品孵育时间和纤维暴露时间。发现的最佳值为 250°C 的样品孵育温度和 30 分钟的孵育和提取时间。PA 纤维不适合极性较弱的邻苯二甲酸酯，因为其萃取和重复性值较差。PDMS 纤维对一些较重的非极性邻苯二甲酸酯的响应很差，而 DVB/CAR/PDMS 纤维对大多数研究的邻苯二甲酸酯表现出最佳的响应和重复性值。所提出的分析方法的主要优点是无需样品处理，从而避免了玻璃器皿、环境、溶剂和样品可能带来的污染。
