Eastern Analytical Symposium & Exposition 2024 Abstract Book

Significance of the topic

The 2024 Eastern Analytical Symposium abstracts illustrate the breadth of modern analytical chemistry across pharmaceutical, biopharmaceutical, environmental, forensic, materials, and food/consumer-product applications. The collection emphasizes three cross-cutting drivers: (1) sensitivity and specificity to detect trace and complex analytes (PFAS, nitrosamines, sub-visible particulates, protein biomarkers, oligonucleotides, viral assemblies), (2) speed and throughput for discovery, process development, and regulatory screening (high-throughput MS, acoustic and acoustic-ejection MS, online PAT), and (3) sustainability and robustness in routine workflows (green sample prep, solvent minimization, improved chromatographic efficiency). These directions reflect real-world needs: ensuring product safety, accelerating drug discovery and scale-up, and monitoring pervasive environmental contaminants.

Objectives and overview of the program

• Survey and synthesize recent methodological advances presented at EAS 2024: novel MS modalities, NMR innovations, chromatography improvements, vibrational and hyperspectral imaging, and microfluidics/miniaturized workflows.
• Highlight targeted application areas: vaccines and biologics characterization, oligonucleotide/siRNA analytics, ADC and peptide manufacturing control, PFAS detection and mass balance, forensic and cultural-heritage analysis, and biomarker discovery for cancer.
• Identify practical themes: assay validation and regulatory alignment (ICH Q14, USP), automation and digital tools (qQMSA, ML), and sustainability in laboratory practice.

Methodologies and analytical approaches reported

• Mass spectrometry enhancements
  • Charge detection MS (CD-MS) for megadalton particles (viruses, VLPs, gene therapy vectors) giving single-ion charge and mass distributions and enabling coupling to chromatographic separations.
  • Acoustic ejection and acoustic ejection MS (AEMS) and DESI-based automated ambient platforms for ultrahigh-throughput reaction screening and biological assays (sub-second to second sampling rates), integrating robotics, high-density arrays, and MS detectors (QQQ, QTOF).
  • Droplet-APCI and FIA-MS approaches for rapid enzymatic reaction screening and terpene detection, with throughputs of tens of seconds per sample and agreement with GC-MS.
  • Coulometric mass spectrometry (CMS) enabling absolute peptide/protein quantitation without isotope-labeled standards via electrochemical oxidation yield measurements coupled to MS.
  • Headspace molecular rotational resonance (MRR) spectroscopy for fast, matrix-independent quantitation of volatile and semi-volatile compounds otherwise hard to analyze by GC.
• Chromatography and separation science
  • Two-dimensional LC workflows (2D-LC, SEC-SEC) and tandem-column liquid chromatography to extend peak capacity and resolve complex vaccine and biotherapeutic mixtures; online coupling to MALS and dRI for absolute MW.
  • New stationary phases and particle technologies: monodisperse fully porous particles (MFPP) for improved metabolomics separations; superficially porous particle (SPP) scalability and solid-core particle options; hybrid silica end-capped with bidentate reagents for high-pH stability; new capillary C18/carbon/HILIC columns for bioanalysis.
  • Hydrophilic interaction (HILIC) and ion-pair RP-LC methods for oligonucleotide separations and PFAS analyses; strategies to mitigate non-specific metal binding for metal-sensitive analytes (MaxPeak HPS).
• Nuclear magnetic resonance (NMR)
  • i-HMBC (isotope-shift-detecting HMBC) to distinguish 2-bond vs longer-range 1H-13C correlations enabling structure elucidation of proton-deficient natural products at sub-mg scale and providing an isotope-shift-based complementary structural strategy.
  • Advances in qNMR: novel universal and tunable internal standards (2,2-difluoroacetamide, DFA), efforts toward platform qNMR methods to enable novices, and automation via qQMSA digital products to speed 1H qNMR analysis.
  • Arrayed spin-lock 1D TOCSY/TOCSY-DEPT for structural assignments, and microfluidic modulation spectroscopy for gRNA higher-order structure probing.
• Vibrational and photothermal spectroscopies
  • Near-field and hyperspectral infrared and Raman imaging enabling nanoscale vibrational mapping (<10–20 nm) of biological samples and materials.
  • Optical photothermal infrared (O-PTIR) and submicron IR (O-PTIR) for chemical identification of sub-visible particulates in biopharmaceuticals, overcoming fluorescence and sensitivity limits of Raman.
  • Widefield fluorescence-detected photothermal IR (FE-PTIR) for chemical imaging of autofluorescent biomaterials and live organisms.
• Specialized methodologies and applications
  • Charge and oxidation studies of technetium in nuclear reprocessing conditions; radiolysis impacts on pertechnetate speciation and extractability.
  • Singlet oxygen photooxidation studies at particle interfaces, and biomimetic oxidation leading to natural-product-like dihydrobenzofurans.
  • Use of SERS for ultra-sensitive PFAS detection in water (femtomolar sensitivity demonstrated) and combustion ion chromatography (CIC, EPA Method 1621) for total fluorine/AOF measurements and PFAS non-target screening.

Principal results and discussion

• Analytical reach expanded: CD-MS has matured to allow chromatography timescale coupling for VLP/virus mass-distribution analysis and stoichiometry optimization; O-PTIR and FE-PTIR enable submicron chemical identity for particulates and live-cell chemical imaging.
• Throughput and automation gains: AEMS, acoustic-ejection, and DESI-MS platforms demonstrate orders-of-magnitude throughput improvements versus traditional LC-MS, enabling screening of large libraries and HTS applications with minimal sample prep.
• Improved robustness and method transfer: Novel chromatographic packings (solid-core, MFPP, high-pH hybrid silica) and surface-passivated hardware address longstanding stability and metal-binding problems for oligonucleotides and polar analytes, facilitating LC-MS compatibility and method scalability.
• qNMR evolution: DFA demonstrates a broadly soluble, tunable internal standard applicable across solvents and matrices; automated digital qNMR analysis (qQMSA) and community efforts toward a platform method aim to broaden qNMR adoption and reproducibility.
• PFAS mass balance and unknown fluorine: LC-HRMS plus TOP and CIC analyses of AFFFs revealed many previously undocumented PFAS classes; total fluorine approaches are key to closing fluorine mass balance and informing regulatory and remediation strategies.
• Regulatory and quality emphasis: Several abstracts focus on practical validation and control strategies (ICH Q14, USP <232>/<233> alignment, method lifecycle), demonstrating how advanced analytical development is being operationalized for compliance and product safety.

Practical benefits and applications of presented methods

• Biopharma: online UHPLC PAT and continuous SPPS/LPPS enable process control and impurity management for peptide manufacture (tirzepatide example); SEC-SEC-MALS workflows accelerate size-distribution and MW characterization for vaccines and complex biologics.
• Drug discovery and HTS: acoustic ejection MS and ambient DESI platforms provide rapid reaction screening and label-free bioassays to speed medicinal chemistry and enzyme evolution programs.
• Safety and regulatory screening: satellite laboratory programs and handheld/portable spectrometers allow targeted on-site screening of unknown drug products and rapid interdiction; validated ICP-MS and CIC workflows support ICH/USP elemental and PFAS requirements.
• Environmental and remediation: SERS and LC-MS/MS/ICP-MS approaches advance PFAS detection in water and matrices, and biowaste adsorbents demonstrate low-cost remediation options for metal ions (Pb, Cd).
• Forensic and cultural heritage: single-molecule blinking-based ML identification of dyes, and multimodal vibrational microscopy, provide nondestructive, high-specificity tools for provenance and forensic inquiries.

Instrumentation used (representative list cited in abstracts)

• Mass spectrometers: QTOF, QQQ triple-quadrupole, high-resolution LC-HRMS, charge-detection MS, ambient DESI-MS, AEMS (Echo systems), droplet-APCI-MS, transportable/handheld MS.
• Chromatography systems: UHPLC, online 2D-LC, SEC-SEC columns, capillary LC and nanoLC, GC×GC, GC-MS with spectral deconvolution and retention-index workflows, headspace-GC approaches.
• NMR: high-field 1H/13C NMR, i-HMBC, arrayed spin-lock TOCSY/DEPT, qNMR platforms, microfluidic modulation spectroscopy (MMS).
• Vibrational and photothermal tools: FTIR, Raman (confocal and resonance), hyperspectral imaging, O-PTIR (optical photothermal IR), FE-PTIR, near-field IR, LDIR imaging, fluorescence lifetime and single-molecule fluorescence setups.
• Other: ICP-MS (NexION 1100), combustion ion chromatography (CIC), molecular rotational resonance (MRR), microfluidic devices, SEM-EDS, cryo-SEM, MALS, dRI detectors, QCM-D, FRAP.

Key contributions and impact for practitioners

• Direct paths to higher-throughput and more sustainable analytics: several methods reduce solvent use, sample volumes, and manual steps while increasing information content (e.g., online PAT, capillary LC, AEMS).
• Improved confidence for complex analytes: hybrid 2D separations, CD-MS, O-PTIR, and high-resolution MS workflows allow characterization of heterogeneous high-mass assemblies and sub-visible particulates important for safety and quality control.
• Regulatory alignment: practical examples of method development and validation illustrate how to implement ICH Q14 and USP guidance in analytical workflows for pharmaceuticals and biologics.
• Adoption enablers: digital tools (qQMSA), community platform method efforts (qNMR), and passive-surface hardware improvements facilitate method transfer and broader adoption in routine labs.

Future trends and potential applications

• Greater integration of automation, robotics, and AI/ML into analytical pipelines—closing the loop between reaction optimization, analytics, and decision-making (self-optimizing flow reactors, ML-driven spectral and image analysis).
• Expansion of ambient and label-free MS (AEMS, DESI, droplet APCI) across HTS, reaction scouting, and process analytics to reduce sample prep burdens.
• Standardization and adoption of total-fluorine and non-targeted PFAS analysis (CIC, TOP assay, LC-HRMS) to support environmental mass-balance and regulatory needs.
• Continued development of hybrid, orthogonal multimodal characterization (NMR + CD-MS + cryo-EM, O-PTIR + Raman + fluorescence) for complex biologics and nanomaterials.
• Widened use of green analytical chemistry practices in forensic and routine lab settings (greener solvents, miniaturization, waste reduction), plus validated microsampling options for patient-centric clinical studies.

Conclusions

The 2024 EAS abstracts underscore a multi-disciplinary push in analytical chemistry toward higher sensitivity, greater throughput, and more sustainable, robust assays across pharmaceuticals, environmental science, and forensic applications. Innovations in MS modalities, chromatography materials and configurations, NMR methodology, and vibrational imaging are converging with automation and computational tools to deliver practical solutions for real-world analytical challenges. For laboratories and R&D groups, the major takeaway is that strategically combining orthogonal techniques, embracing automation, and designing for regulatory robustness will accelerate both discovery and reliable product delivery.

References (selected citations mentioned in abstracts)

• Winston A., Sustainable Business Went Mainstream in 2021, Harvard Business Review, Dec. 2021.
• Liu Z. and Foley J. Chromatographia/ J. Chromatogr. A, 2022. DOI:10.1016/j.chroma.2022.462890 (tandem-column LC review).
• Krishnamurthy, K., CRAFT/CRAFT-NMR and CRAFT-related NMR analysis methods, Magn. Reson. Chem., 2013, 51, 821–829.
• Lodge S. et al., Methods for suppression/advanced NMR experiments, Anal. Chem., 2021, 93, 3976–3986.
• Nitschke P. et al., Advanced NMR suppression techniques, Anal. Chem., 2022, 94, 1333–1341.
• Fuertes-Martín R., Correig X., Vallvé J.C., Amigó N., GlycA/GlycB clinical NMR biomarkers, Life, 2021, 11, 1407.
• EPA Method 1621: Determination of Adsorbable Organic Fluorine (AOF) in Aqueous Matrices by Combustion Ion Chromatography (finalized Jan 2024).