Department of Analytical Chemistry, Faculty of Chemistry, Universitat de València, Dr Moliner 50, 46100, Burjassot, Valencia, Spain.
Institute of Material Science (ICMUV), Universitat de València, Catedrático José Beltrán 2, 46980 Paterna, Valencia, Spain.
J Chromatogr A. 2021 Feb 22;1639:461938. doi: 10.1016/j.chroma.2021.461938. Epub 2021 Jan 23.
A sorbent for the extraction of organophosphorus flame retardants has been proposed, based on UVM-7 (University of Valencia Materials) mesoporous silica doped with titanium. Designed cartridges have been applied to the extraction and preconcentration of flame retardants in water samples, followed by gas chromatography coupled to a mass spectrometry detector. Firstly, UVM-7 materials with different contents of titanium were synthesized and characterized by several techniques, thus confirming the proper mesoporous architecture. The potential of these materials was assessed in comparison with their morphological properties, resulting Ti50-UVM-7 the best solid phase. Several extraction parameters were also optimized. Analytical parameters were also evaluated, and limits of detection from 0.019 to 0.21 ng mL were obtained, as well as intra-day relative standard deviation below 11% for all analytes. Extraction efficiencies above 80% in water samples were achieved. The reusability of the material was also proved. Finally, the designed protocol was applied for the analysis of real water samples, and quantifiable concentrations of tris(2-chloroisopropyl) phosphate (TCIPP), tris(1,3-dichloro-2-propyl) phosphate (TDCIPP) and triphenyl phosphate (TPhP) were obtained in some samples. The method was compared with a United States Environmental Protection Agency general method with C18 cartridges.
一种基于掺杂钛的巴伦西亚大学材料（UVM-7）介孔硅的有机磷阻燃剂萃取吸附剂已被提出。设计的试剂盒已应用于水样中阻燃剂的萃取和预浓缩，随后进行气相色谱-质谱联用检测。首先，通过多种技术合成并表征了不同钛含量的 UVM-7 材料，从而证实了其具有适当的介孔结构。通过比较这些材料的形态特性评估了它们的潜在性能，结果表明 Ti50-UVM-7 是最佳的固相。还优化了几种萃取参数。评估了分析参数，对于所有分析物，检测限在 0.019 至 0.21 ng mL 之间，所有分析物的日内相对标准偏差均低于 11%。在水样中实现了 80%以上的萃取效率。还证明了该材料的可重复使用性。最后，该设计方案已应用于实际水样的分析，在一些样品中可定量检测到三（2-氯异丙基）磷酸酯（TCIPP）、三（1,3-二氯-2-丙基）磷酸酯（TDCIPP）和三苯基磷酸酯（TPhP）的浓度。该方法与美国环保署使用 C18 试剂盒的一般方法进行了比较。
