Kesic Blake, McCann Niamh, Bowerbank Samantha L, Standley Troy, Liechti Jana, Dean John R, Gallidabino Matteo D
Department of Applied Sciences, Northumbria University, Newcastle Upon Tyne, NE1 8ST, UK.
King's Forensics, Department of Analytical, Environmental & Forensic Sciences, King's College London, London, SE1 9NH, UK.
Anal Bioanal Chem. 2024 Mar;416(8):1907-1922. doi: 10.1007/s00216-024-05189-w. Epub 2024 Feb 9.
Smokeless powders (SLPs) are composed of a combination of thermolabile and non-thermolabile compounds. When analysed by GC-MS, injection conditions may therefore play a fundamental role on the characterisation of forensic samples. However, no systematic investigations have ever been carried out. This casts doubt on the optimal conditions that should be adopted in advanced profiling applications (e.g. class attribution and source association), especially when a traditional split/splitless (S/SL) injector is used. Herein, a study is reported that specifically focused on the evaluation of the liner type (L) and inlet temperature (T). Results showed that both could affect the exhaustiveness and repeatability of the observed chemical profiles, with L being particularly sensitive despite typically not being clarified in published works. Perhaps as expected, degradation effects were observed for the most thermolabile compounds (e.g. nitroglycerin) at conditions maximising the heat transfer rates (L = packed and T ≥ 200 °C). However, these did not seem to be as influential as, perhaps, suggested in previous studies. Indeed, the harshest injection conditions in terms of heat transfer rate (L = packed and T = 260 °C) were found to lead to better performances (including better overall %RSDs and LODs) compared to the mildest ones. This suggested that implementing conditions minimising heat-induced breakdowns during injection was not necessarily a good strategy for comparison purposes. The reported findings represent a concrete step forward in the field, providing a robust body of data for the development of the next generation of SLP profiling methods.
无烟粉末(SLP)由热不稳定和非热不稳定化合物组合而成。因此,在通过气相色谱 - 质谱联用(GC-MS)分析时,进样条件可能对法医样本的特征描述起着至关重要的作用。然而,从未进行过系统的研究。这使得人们对高级分析应用(如类别归属和来源关联)应采用的最佳条件产生怀疑,尤其是在使用传统分流/不分流(S/SL)进样器时。本文报道了一项专门针对衬管类型(L)和进样口温度(T)评估的研究。结果表明,两者都会影响所观察到的化学图谱的详尽程度和重复性,尽管在已发表的作品中通常未明确说明,但衬管类型尤为敏感。也许正如预期的那样,在使传热速率最大化的条件下(L = 填充型且T≥200°C),观察到了对最热不稳定化合物(如硝酸甘油)的降解作用。然而,这些影响似乎并不像先前研究中所暗示的那样具有影响力。事实上,就传热速率而言,发现最严苛的进样条件(L = 填充型且T = 260°C)与最温和的条件相比,能带来更好的性能(包括更好的总体相对标准偏差和检测限)。这表明,在进样过程中实施使热诱导分解最小化的条件,对于比较目的而言不一定是一个好策略。所报道的研究结果代表了该领域向前迈出的具体一步,为下一代SLP分析方法的开发提供了强大的数据支持。