Franchina Flavio A, Zanella Delphine, Dejong Thibaut, Focant Jean-François
Molecular System, Organic & Biological Analytical Chemistry Group, University of Liège, Liège, Belgium.
Molecular System, Organic & Biological Analytical Chemistry Group, University of Liège, Liège, Belgium.
Talanta. 2021 Jan 15;222:121569. doi: 10.1016/j.talanta.2020.121569. Epub 2020 Aug 27.
The increased attraction of biological volatile compounds has opened the route to a wide variety of sampling techniques, amongst which trap tubes packed with adsorbent materials are commonly used. Many types of adsorbent materials are available and the choice of the adsorbent can impact the obtained results in untargeted analysis. Therefore, a proper combination of the adsorbent material and the sample is necessary to increase the robustness and reproducibility of biological studies. In this study, the sampling performance of thermal desorption tubes with six common adsorbent material combinations, i.e., Tenax® TA, Tenax® TA/Carbopack™ B, Tenax® TA/Sulficarb, Tenax® TA/Carbograph™ 5TD, Tenax® TA/Carbograph™ 1TD/Carboxen® 1003, and Carboxen® 1016/Carbograph™ 5TD, was evaluated in two different setups: in vitro and in vivo sampling. The in vitro setup consisted of the headspace dynamic extraction of spiked serum, and a mixture of 19 standards was evaluated in terms of response and reproducibility. The in vivo setup consisted into two parts: the first one was based the evaluation of the standard mixture, which was flash-vaporised into Tedlar® bags containing exhaled breath; the second part was based on the longitudinal monitoring of breath metabolites originating from a beverage intake (i.e., brewed coffee), over a 90 min time period. The tubes were all desorbed and analysed in a comprehensive two-dimensional gas chromatography system coupled to a high-resolution time-of-flight mass spectrometer (GC × GC-HR ToF MS). In both sampling setups, the widest analytes coverage and the overall best extraction yield on the selected compounds were obtained using Tenax® TA, followed by Tenax® TA/Carbopack™ B. Tenax® TA provided the highest sampling reproducibility with 12 %RSD, 10 %RSD and <5 %RSD of the response during the experiments using the in vitro setup, the in vivo setup, and during the longitudinal tracking, respectively.
生物挥发性化合物吸引力的增加开启了通往多种采样技术的道路，其中填充吸附材料的捕集管是常用的。有许多类型的吸附材料可供选择，吸附剂的选择会影响非靶向分析中获得的结果。因此，吸附材料和样品的适当组合对于提高生物学研究的稳健性和可重复性是必要的。在本研究中，评估了六种常见吸附材料组合的热脱附管的采样性能，即Tenax® TA、Tenax® TA/Carbopack™ B、Tenax® TA/Sulficarb、Tenax® TA/Carbograph™ 5TD、Tenax® TA/Carbograph™ 1TD/Carboxen® 1003和Carboxen® 1016/Carbograph™ 5TD，采用两种不同的设置：体外和体内采样。体外设置包括加标血清的顶空动态萃取，并根据响应和重现性评估了19种标准物的混合物。体内设置分为两部分：第一部分基于对标准混合物的评估，该混合物被闪蒸到含有呼出气体的Tedlar®袋中；第二部分基于对饮料摄入（即煮咖啡）产生的呼吸代谢物在90分钟时间段内的纵向监测。所有的管子都在与高分辨率飞行时间质谱仪联用的全二维气相色谱系统（GC × GC-HR ToF MS）中进行脱附和分析。在两种采样设置中，使用Tenax® TA获得了最宽的分析物覆盖范围和对所选化合物的总体最佳萃取产率，其次是Tenax® TA/Carbopack™ B。在使用体外设置、体内设置和纵向跟踪的实验过程中，Tenax® TA分别提供了最高的采样重现性，响应的相对标准偏差（RSD）分别为12%、10%和<5%。
