14th Multidimensional Chromatography Workshop Guidebook

Význam tématu

Comprehensive two-dimensional chromatography (both GC×GC and LC×LC) addresses the growing need for resolving highly complex mixtures that are commonplace in environmental analysis, fuels, foodomics, pharmaceutical quality control and forensic investigations. By dramatically increasing peak capacity and enhancing selectivity, these techniques enable the detection and quantitation of trace compounds that would remain hidden in conventional one-dimensional separations. The workshop highlighted how multidimensional separations combined with advanced detection and data analysis unlock new insights across disciplines.

Cíle a přehled konference

The 14th Multidimensional Chromatography Workshop convened experts to share recent advances and applications of GC×GC, LC×LC, hybrid methods, novel modulators and chemometric tools. Key objectives included:

• Showcasing innovative modulator designs (thermal, flow, active solvent) and microfluidic architectures
• Exchanging best practices for method development and automation in heart-cut and comprehensive instruments
• Demonstrating applications to plastic-derived fuel characterization, fruit volatile profiling, adhesives in archaeology, bio-oils, and pharmaceutical complex drugs
• Discussing new computational workflows, AI-driven pattern recognition, simulation platforms and software for multidimensional data mining

Použitá metodika a instrumentace

Participants presented a broad range of instrumental setups and sampling strategies, including:

• GC×GC with cryogenic and flow modulators, combined with TOF-MS, QqQ-MS, VUV or dual TOFMS/FID detection
• LC×LC with active solvent modulation to bridge incompatible mobile phases (e.g., HILIC×RPLC)
• Microfluidic prototypes for spatial multidimensional LC fabricated by DLP 3D-printing
• Temperature-responsive 1D LC coupled to ultrafast chiral RPLC for enantiomeric separations
• Automated LC-GC×GC hyphenation platforms for mineral oil quantitation (MOSH/MOAH) using parallel FID and ToFMS detection
• Sample enrichment techniques: SPME, HiSorb™, thermal desorption (TD), vacuum-assisted headspace, multi-cumulative trapping
• Dedicated software: AnalyzerPro XD for MS deconvolution; GC Image MDC Investigator™ for peak alignment, PCA, Fisher ratio analysis and machine learning
• Modulation and connectivity hardware: SilFlow® microfluidic connectors, SilTite® ferrules, Trajan SGE inlet liners and CRS septa, wide range of Supelco and Trajan GC columns
• High-resolution TOF-MS systems (30 000 resolving power, 1 ppm accuracy) with multiple ion sources (EI, CI, PI, FI, FD)

Hlavní výsledky a diskuse

Key findings and discussions encompassed:

• Quantitative analysis of aliphatic olefins up to C25 at wt.% levels in fuels from plastic waste via GC×GC-FID and DMDS derivatization
• Automated unsupervised optimization algorithms for 2D-LC method development and the current challenges in scaling to heart-cut and comprehensive modes
• Flow-modulated GC×GC-MS/FID simplifies routine petroleum group-type quantitation (ASTM D8396 workflow)
• Microfluidic spatial MD-LC devices enabling parallel IEF×SEC separations of intact proteins in single analysis
• Hyphenation of temperature-responsive LC with ultrafast chiral RPLC for generic enantiomeric screening in pharmaceuticals
• Use of GC×GC-TOFMS/FID in mineral oil analysis improved specificity and robustness compared to 1D methods
• Identification of over 400 volatile compounds in complex matrices (whisky, olive oil, beer, coffee, fruit) using SPME/TD–GC×GC–TOFMS with tile-based chemometrics
• Non-destructive headspace sampling for volatile adhesives, body odor and microbiological screening in food and forensic applications
• Modular simulation tools and big-data driven retention modelling for virtual prototyping of complex GC and GC×GC systems
• Advances in alignment and feature discovery for multilayered 4D GC3-TOFMS data using extended tile-based Fisher ratio analysis

Přínosy a praktické využití metody

Comprehensive multidimensional chromatography has demonstrable benefits in:

• Petroleum and alternative fuel characterization: detailed profiling of alkanes, aromatics, sulfur and polar oxygenates for quality and performance correlations
• Food and beverage authenticity and quality control: fingerprinting of olive oils, whiskies, lagers and fruit aromas to monitor spoilage, origin and processing
• Pharmaceutical analytics: deeper understanding of complex drug formulations (e.g., sodium bituminosulfonate, monoclonal antibodies) through targeted and untargeted 2D separations
• Forensics and health monitoring: rapid GC×GC-based volatile marker detection for decomposition odor, body odor biomarkers, and microbial contaminants in food
• Environmental and agricultural: analysis of biocrude from straw pyrolysis, pesticide panels in complex food matrices, gas phase contaminants in renewable gases

Budoucí trendy a možnosti využití

Emerging directions include:

• Integration of AI and computer vision workflows for chromatographic image fingerprinting and non-target feature discovery
• Wider adoption of high-resolution TOF and FT-MS detectors with soft ionization to improve speciation of sulfur and nitrogen compounds
• Green and high-throughput sample preparation using automated SPME/TD systems and microfluidic modulators
• Expansion of spatial multidimensional separations in LC×LC and GC×GC to new sample classes via digital 3D-printing
• Robust in silico simulation platforms for method optimization and virtual instrument prototyping to reduce development time
• Standardization of GC×GC methods in regulated industries (e.g., petroleum ASTM protocols) and interlaboratory harmonization

Závěr

The workshop underscored that comprehensive two-dimensional chromatography has matured into a versatile, high-performance platform across diverse fields. Continued development of automated method development tools, high-resolution detectors, advanced sampling interfaces and AI-driven data analytics will accelerate its integration into routine analysis. Collaboration across academia, instrument vendors and end-users remains critical to remove barriers, standardize protocols and expand the adoption of multidimensional separations.

Reference

None provided in original text.