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Sorbent coatings for solid-phase microextraction targeted towards the analysis of death-related polar analytes coupled to comprehensive two-dimensional gas chromatography: Comparison of zwitterionic polymeric ionic liquids versus commercial coatings
Microchemical Journal ( IF 4.9 ) Pub Date : 2020-11-01 , DOI: 10.1016/j.microc.2020.105243
Íris R. Carriço , Jéssica Marques , Maria J. Trujillo-Rodriguez , Jared L. Anderson , Sílvia M. Rocha

Abstract Decomposition of bodies generates several types of polar volatile organic compounds (VOCs), whose types, patterns and ratios change during the various stages of decomposition and, therefore, their determination has huge potential to provide useful information to disclose events related to the time of death, or body surrounding environment. As sample preparation is a mandatory key-point in a method development, this research aims to develop a simple, accurate and rapid approach to study death-related polar VOCs based on headspace solid-phase microextraction (HS-SPME) combined with comprehensive two-dimensional gas chromatography-time of flight mass spectrometry (GC × GC-ToFMS) analysis. The performance of zwitterionic PIL-based fibers (containing a [VIm+C9COO−] monomer and a [(VIm)2C122+]-2Br− crosslinker), tailored for polar compounds, was evaluated for a set of 19 analytes associated with the unique odour created by decomposing bodies, and it was compared to the commercially-available fibers: divinylbenzene/carboxen/poly(dimethylsiloxane) – DVB/CAR/PDMS, poly(dimethylsiloxane)/divinylbenzene – PDMS/DVB and polyacrylate (PA). Fibers with absorptive-type mechanism, such as PA and PIL, showed the best results in the balance of the parameters studied, being able to detect analytes at ng level and providing a profile representative of the headspace composition, thus they may represent a useful tool to respond to current challenges in forensic taphonomy. The reproducibility (with relative standard deviation lower than 18%, depending on the analyte) and relative recoveries (higher than 99.1%) were similar and acceptable for both fibers. The zwitterionic PIL, with ca. 4 times smaller film thickness than PA, still has potential to have the best performance, supported by the efforts to obtain thicker sorbent coatings.

中文翻译:

用于分析死亡相关极性分析物的固相微萃取吸附剂涂层与综合二维气相色谱联用:两性离子聚合物离子液体与商业涂层的比较

摘要 尸体分解会产生多种极性挥发性有机化合物 (VOC),其类型、模式和比例在分解的各个阶段都会发生变化,因此,它们的测定具有巨大的潜力,可以为揭示与时间相关的事件提供有用的信息。死亡,或身体周围的环境。由于样品制备是方法开发的一个强制性关键点,本研究旨在开发一种简单、准确、快速的方法,基于顶空固相微萃取 (HS-SPME) 结合综合两维气相色谱-飞行时间质谱 (GC × GC-ToFMS) 分析。基于两性离子 PIL 的纤维(含有 [VIm+C9COO−] 单体和 [(VIm)2C122+]-2Br− 交联剂)的性能,专为极性化合物而设计,对一组 19 种分析物进行了评估,这些分析物与分解尸体产生的独特气味相关,并将其与市售纤维进行比较:二乙烯基苯/羧基/聚(二甲基硅氧烷)– DVB/CAR/PDMS、聚(二甲基硅氧烷)/二乙烯基苯– PDMS/DVB 和聚丙烯酸酯 (PA)。具有吸收型机制的纤维,如 PA 和 PIL,在研究参数的平衡方面表现出最好的结果,能够检测 ng 水平的分析物并提供代表顶空组成的轮廓,因此它们可能是一种有用的工具以应对法医埋藏学当前的挑战。两种纤维的重现性(相对标准偏差低于 18%,取决于分析物)和相对回收率(高于 99.1%)相似且可接受。两性离子 PIL,约。
更新日期:2020-11-01
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