In this study, the scientists aimed to create a workflow that allows for the simultaneous separation and detection of inorganic anions, cations, and organic explosive materials from a single injection. A heart-cutting two-dimensional liquid chromatography (2D-LC) method was used in this process. In the first dimension, hydrophilic interaction chromatography (HILIC) was applied for the separation of inorganic anions and cations. Using active solvent modulation enabled the organic fraction to be transferred and refocused on in the second dimension, which involved reversed-phase LC (RPLC) separation.
To test this analysis strategy, the system was used to detect ammonium. To enable sensitive detection, a derivatization protocol was developed. The mobile phases of both separation dimensions were compatible with MS, allowing for notably sensitive detection and selective, admissible identification. Overall, a combination of evaporative light scattering and ultraviolet (UV) absorption was used to detect all the analytes, with UV spectra helping to distinguish between organic explosives.
Future work may implement MS detection into 1D HILIC to solve the problems of analyte identification and poor detection limits of technologies like evaporative light scattering detectors (ELSDs). However, this would involve MS having to switch between positive and negative mode rapidly as the inorganic analytes possess both charge states. Ultimately the scientists declared their 2D-LC method to be applicable to pre- and post-blast explosive materials that may be collected as physical evidence at crime scenes. Achieving this requires the investigation of different matrices’ influences in which explosive residues may be present at crime scenes. Tentatively using MS detection will be even more important for practically applying this separation method and identifying peaks, regardless of retention time or UV absorbance spectrum, before the method goes through validation.
Reference
(1) Hurk, R. S. v. d.; Belina, E.; Verduin, J.; et al. Simultaneous Analysis of Organic and Inorganic Explosive Traces by Online Two-Dimensional Liquid Chromatography. J. Chromatogr. A 2025, 1758, 466187. DOI: 10.1016/j.chroma.2025.466187