16th Multidimensional Chromatography Workshop Abstract book

Summary of the Workshop on Advanced Multidimensional Chromatography (Feb 3–5, 2025)

Importance of the Topic

The ability to resolve, identify and quantify complex mixtures underpins modern analytical science. Multidimensional separation techniques—comprehensive two-dimensional gas chromatography (GC×GC) and two-dimensional liquid chromatography (LC×LC), as well as multidimensional supercritical fluid chromatography (SFC×SFC) and emerging 3D spatial LC—extend the peak capacity, sensitivity and selectivity far beyond one-dimensional methods. These advances are driving breakthroughs across environmental monitoring, food and flavor profiling, pharmaceutical and biopharmaceutical analysis, forensic investigations, and quality control in industrial processes.

Objectives and Workshop Overview

This workshop brought together academic and industrial experts to present recent innovations in instrumentation, sampling strategies, data processing and real-world applications of GC×GC, LC×LC, SFC×SFC and related multidimensional techniques. Presentations covered method development, modulation hardware, source-targeted and non-targeted screening, and case studies spanning bio-oil characterization, fragrance allergen analysis, peptide impurity profiling, microplastic leachate screening, volatile biomarker discovery, and more.

Methodology and Instrumentation

• Chromatographic Platforms: GC×GC-TOFMS (thermal and flow modulated), GC×GC-QMS/FID, 1D GC-VUV, LC×LC coupled to high-resolution mass spectrometry (HRMS), multidimensional SFC×SFC, and emerging spatial 3D-LC microchips.
• Ionization Sources: Electron ionization (EI), soft EI (10–12 eV), positive and negative chemical ionization (PCI, NCI), photoionization (PI), field ionization (FI), and dual-source ESI/TPI for LC–MS.
• Sampling & Sample Prep: Headspace SPME/HS-SPE/DHS, thermal desorption, microwave-assisted extraction and derivatization (MAED), pressurized liquid extraction (PLE), microwave-assisted saponification/extraction (MASE), pyrolysis probes, TwinBridge push-pull interfaces, multi-heart-cut and comprehensive modulation strategies (SPAM, ASM, at-column dilution).
• Data Processing: Automated peak detection and alignment (PARAFAC-based, tile-based, pixel-based, Pearson correlation for fingerprinting), open-source software modules, chemometric workflows (PCA, PLS-DA), AI-driven pattern recognition, retention index and mass defect plotting.

Main Results and Discussion

• Environmental Analysis: Non-targeted PFAS profiling in water and fluoropolymer leachate with GC×GC-HRToFMS; ultrafine particle PAH speciation; bio-oil composition and upgrading (bio-resins, pyrolysis oils); VOC profiling for packaging migration into oats; air quality improvement studies in mining and informal settlements; untargeted metabolomic/exposomic screening in wastewater and soil; microplastic‐associated chemicals in marine environments.
• Food and Flavor: Comprehensive volatile fingerprinting in oolong teas, hazelnuts, garlic, pistachio, Valcasotto cheese, poi, and honey; targeted allergen quantification in essential oils; terpenoid and carotenoid-derived aroma enantiomer analysis; integration of multisource data for quality and authenticity assessment.
• Pharmaceutical & Biotech: 2D-LC-MS for peptide impurity and peak purity analysis with salt-based eluents; profiling of monoclonal antibody structure/function via multidimensional affinity chromatography and mass spectrometry; characterizing therapeutic AAV capsid variants and PTMs by SEC-UV-RP-MS; lipid and sterol analysis in pharmaceutical formulations.
• Forensic & Public Health: Body odor (cutaneous volatilome) sampling with SkinVOCs® for non-invasive health screening; firearm cartridge scent analysis; fingerprint residue optimization via GC×GC; breath VOC sampling standardization with the Peppermint Initiative; mold detection in materials; headspace profiling for fire debris and chemical threat detection; cork taint in wine; third-hand exposure from textiles.
• Fundamental & Technical Advances: Design of microcolumns (NEMS, radially-elongated pillars) for miniaturized GC×GC; development of spatial 3D-LC microchips for intact protein analysis; push-pull interfaces for 2D-LC; dual-source Q-ToF MS; high-throughput multi-channel ACC metabolite extraction; immersive VR/AR data visualization; automated closed-loop method optimization integrating retention modeling and Bayesian optimization.

Benefits and Practical Applications

The presented methods deliver unparalleled ability to deconvolute complex mixtures, enabling reliable non-target screening, regulatory compliance (e.g. fragrance allergens, PAHs, MOSH/MOAH), process monitoring (bio-fuel and pyrolysis upgrading), food authenticity and spoilage diagnostics, exposome‐based health assessments, quality-control of pharmaceuticals and biologics, roadway and occupational air monitoring, and forensic identification without destructive sampling.

Future Trends and Possibilities

• Integration of machine learning and AI for automated peak detection, spectral annotation, anomaly detection, and predictive maintenance.
• Further miniaturization of multidimensional systems (microfluidic chips, portable GC×GC, on-site SPME-GC×GC workflows) for field applications and space exploration.
• Spatial 3D-LC and hyphenation with ion mobility for ultra-high peak capacities in proteomics and environmental screening.
• Real-time closed-loop optimization of multidimensional methods leveraging retention modeling, chemometrics, and automated hardware feedback.
• Advanced data visualization (immersive, VR/AR) and open-source software platforms for democratized access and community‐driven method development.

Conclusion

The workshop underscored the transformative power of multidimensional separations paired with high-resolution detection and advanced data analytics. By combining novel sample preparation strategies, cutting-edge hardware, and next-generation data processing, practitioners can tackle ever more complex analytical challenges—ranging from trace pollutants in the environment to subtle biomarker shifts in health and disease—paving the way toward more sensitive, selective, and sustainable analytical solutions.

References

Key literature and standards cited across presentations include regulatory methods (e.g. ISO 20122, EU 2023/1545, IFRA methods), seminal patents (WO2017207467A1), and peer-reviewed studies on GC×GC applications in metabolomics, food and environmental analysis, pharmaceutical characterizations, and forensic science.