Bou Saad Maria, Ravier Sylvain, Durand Amandine, Temime-Roussel Brice, Gaudefroy Vincent, Pevere Audrey, Wortham Henri, Doumenq Pierre
LCE, Aix Marseille University, 13331 Marseille, France.
Materials for Transportation Infrastructures Laboratory (MIT), Materials and Structures Department (MAST), Université Gustave Eiffel, Allée des Ponts et Chaussées, CS4, 44344 Bouguenais, France.
Molecules. 2025 Aug 16;30(16):3397. doi: 10.3390/molecules30163397.
Polycyclic aromatic hydrocarbon (PAH) derivatives, specifically azaarenes and nitrated and oxygenated PAHs, are emerging contaminants of concern due to their increased toxicity and persistence compared to the parent PAHs. Despite their toxicity, their simultaneous analysis in complex matrices, such as in fumes emitted from bituminous mixtures, remains challenging due to limitations of conventional analytical techniques. To address this, an advanced methodology was developed using Ultra-High-Performance Liquid Chromatography coupled with High-Resolution Mass Spectrometry (UHPLC-HRMS Orbitrap Eclipse) equipped with an APCI source for the simultaneous identification and quantification of 14 PAH derivatives. Chromatographic and ionization parameters were optimized to ensure maximum sensitivity and selectivity. Following ICH Q2(R2) guidelines, the method was validated, demonstrating excellent linearity (R > 0.99), high mass accuracy (≤5 ppm), strong precision (<15%), and excellent sensitivity. Limits of detection (LODs) ranged from 0.1 µg L to 0.6 µg L and limits of quantification (LOQs) ranged from 0.26 µg L to 1.87 µg L. The validated method was successfully applied to emissions from asphalt pavement materials collected on quartz filters under controlled conditions, enabling the identification and quantification of all 14 targeted compounds. These results confirm the method's robustness and suitability for trace-level analysis of PAH derivatives in complex environmental matrices.
多环芳烃（PAH）衍生物，特别是氮杂芳烃以及硝化和氧化的多环芳烃，由于其相较于母体多环芳烃具有更高的毒性和持久性，正成为备受关注的新兴污染物。尽管它们具有毒性，但在复杂基质中，如沥青混合物排放的烟雾中对其进行同时分析，由于传统分析技术的局限性，仍然具有挑战性。为了解决这个问题，开发了一种先进的方法，使用配备大气压化学电离（APCI）源的超高效液相色谱与高分辨率质谱联用仪（UHPLC-HRMS Orbitrap Eclipse），用于同时鉴定和定量14种多环芳烃衍生物。对色谱和电离参数进行了优化，以确保最大灵敏度和选择性。按照国际协调会议（ICH）Q2（R2）指南对该方法进行了验证，结果表明该方法具有出色的线性（R>0.99）、高质量准确度（≤5 ppm）、高精密度（<15%）和出色的灵敏度。检测限（LOD）范围为0.1 μg/L至0.6 μg/L，定量限（LOQ）范围为0.26 μg/L至1.87 μg/L。经过验证的方法成功应用于在受控条件下收集在石英滤纸上的沥青路面材料的排放物分析，能够鉴定和定量所有14种目标化合物。这些结果证实了该方法对于复杂环境基质中多环芳烃衍生物痕量分析的稳健性和适用性。
