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热脱附气相色谱-气相色谱/飞行时间质谱分析前体臭采样的采样阶段研究

Study of sampling phases for body odor sampling prior to analysis by TD-GC×GC/ToFMS.

作者信息

Boudard Elsa, Fisson Lisa, Moumane Nabil, Dugay José, Vial Jérôme, Thiébaut Didier

机构信息

UMR CBI, Laboratoire des Sciences Analytiques, Bioanalytiques et Miniaturisation, ESPCI Paris, PSL Research University, 10 rue Vauquelin, 75231, Paris, Cedex 05, France.

SenseDetect Health-Care, 21 grande rue, 78240, Aigremont, France.

出版信息

Anal Bioanal Chem. 2025 Jun;417(14):3177-3190. doi: 10.1007/s00216-025-05857-5. Epub 2025 Apr 14.

Abstract

Body odor consists of a complex matrix of volatile organic compounds (VOCs), which has garnered increasing interest in fields like medicine for its potential in disease diagnosis. However, the field of body odor analysis is advancing slowly, partly due to a lack of standardized methodologies. Although gas chromatography-mass spectrometry (GC-MS) is widely used for VOC analysis, there is a broad range of sampling and extraction methods, leading to different or even sometimes contradictory results. To move toward standardized procedures, this study compares five sampling phases for direct body odor sampling in terms of analytical cleanliness and VOC trapping/release efficiency: gauze, glass beads, PowerSorb, Getxent microtubes, and passive sampling pillows (PSP). Thermodesorption was employed to simplify the protocol and minimize contamination or sample loss, which often occurs during multistep processes. Given the matrix's complexity and the need to detect trace-level compounds, comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC×GC/ToFMS) was used to achieve high sensitivity and peak capacity. PSP and PowerSorb demonstrated the best performance, with mean recovery yields of 95% and 71%, respectively, and 22% and 10% variability, ensuring good repeatability. These findings, initially obtained under simulated conditions with a synthetic mixture, were validated with real body odor samples, with an optimal sampling duration estimated between 30 min and 1 h. This study not only highlights these effective sampling solutions but also emphasizes the risks associated with using sorbent phases that lack adequate analytical cleanliness (i.e., clean blank) such as gauze.

摘要

体臭由挥发性有机化合物(VOCs)的复杂基质组成,因其在疾病诊断中的潜力而在医学等领域引起了越来越多的关注。然而,体臭分析领域进展缓慢,部分原因是缺乏标准化方法。尽管气相色谱-质谱联用(GC-MS)被广泛用于VOC分析,但存在广泛的采样和提取方法,导致结果不同甚至有时相互矛盾。为了迈向标准化程序,本研究比较了直接体臭采样的五个采样阶段在分析清洁度和VOC捕获/释放效率方面的表现:纱布、玻璃珠、PowerSorb、Getxent微管和被动采样枕(PSP)。采用热脱附来简化方案并最大限度地减少在多步骤过程中经常出现的污染或样品损失。鉴于基质的复杂性以及检测痕量水平化合物的需求,使用全二维气相色谱与飞行时间质谱联用(GC×GC/ToFMS)来实现高灵敏度和峰容量。PSP和PowerSorb表现最佳,平均回收率分别为95%和71%,变异性分别为22%和10%,确保了良好的重复性。这些最初在模拟条件下用合成混合物获得的结果,在真实体臭样品中得到了验证,估计最佳采样持续时间在30分钟至1小时之间。本研究不仅突出了这些有效的采样解决方案,还强调了使用缺乏足够分析清洁度(即清洁空白)的吸附剂相(如纱布)所带来的风险。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/3049/12103381/9651784f7c23/216_2025_5857_Fig1_HTML.jpg

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