Univ. Grenoble Alpes, CEA, LETI, MINATEC Campus, F-38000 Grenoble, France. UMR 8231 CBI, LSABM, ESPCI Paris-CNRS, PSL Institute, Paris, France.
J Breath Res. 2018 Sep 12;12(4):046011. doi: 10.1088/1752-7163/aad384.
This work presents the performances of silicon micro-preconcentrators chips for breath sampling. The silicon chips were coupled to a handheld battery powered system for breath sampling and direct injection in a laboratory gas chromatography mass spectrometry system through thermal desorption (TD). Performances of micro-preconcentrators were first compared to commercial TD for benzene trapping. Similar chromatographic peaks after gas chromatographic separation were observed while the volume of sample needed was reduced by a factor of 5. Repeatability and day to day variability of the micro-preconcentrators were then studied for a 500 ppb synthetic model mixture injected three times a day four days in a row: 8% and 12% were measured respectively. Micro-preconcentrator to micro-preconcentrator variability was not significant compared to day to day variability. In addition, micro-preconcentrators were tested for breath samples collected in Tedlar bags. Three analyses of the same breath sample displayed relative standard deviations values below 16% for eight of the ten most intense peaks. Finally, the performances of micro-preconcentrators for breath sampling on a single expiration were illustrated with the example of volatile tobacco markers tracking. The signals of three smoking markers in breath, benzene, 2,5-dimethylfuran, and toluene were studied. Concentrations of benzene and toluene were found to be 10 to 100 higher in the breath of smokers. 2,5-dimethylfuran was only found in the breath of smokers. The elimination kinetics of the markers were followed as well during 4 h: a fast decrease of the signal of the three markers in breath was observed 20 min after smoking in good agreement with what is described in the literature. Those results demonstrate the efficiency of silicon chips for breath sampling, compared to the state of the art techniques. Thanks to miniaturization and lower sample volumes needed, micro-preconcentrators could be in the future a key technology towards portable breath sampling and analysis.
本工作展示了用于呼吸采样的硅微预浓缩器芯片的性能。硅芯片与手持式电池供电系统耦合,用于通过热解吸 (TD) 在实验室气相色谱质谱系统中进行呼吸采样和直接进样。首先将微预浓缩器的性能与商用 TD 进行了比较,以用于苯的捕获。在进行气相色谱分离后,观察到了相似的色谱峰,而所需的样品体积减少了 5 倍。然后,研究了微预浓缩器在连续四天每天注射三次 500 ppb 合成模型混合物时的重复性和日间变异性:分别测量到 8%和 12%。与日间变异性相比,微预浓缩器之间的变异性不显著。此外,还对 Tedlar 袋中采集的呼吸样本进行了微预浓缩器测试。对同一样本的三次分析显示,对于十个最强峰中的八个,相对标准偏差值低于 16%。最后,以挥发性烟草标志物跟踪为例,说明了微预浓缩器用于单次呼气的呼吸采样性能。研究了呼吸中的三个吸烟标志物苯、2,5-二甲基呋喃和甲苯的信号。发现吸烟者呼吸中的苯和甲苯浓度高 10 至 100 倍。2,5-二甲基呋喃仅在吸烟者的呼吸中发现。还研究了标志物在 4 小时内的消除动力学:吸烟后 20 分钟,呼吸中三种标志物的信号迅速下降,与文献中描述的情况非常吻合。这些结果表明,与现有技术相比,硅芯片在呼吸采样方面具有优势。由于微型化和所需样品量减少,微预浓缩器将来可能成为便携式呼吸采样和分析的关键技术。