EASTERN ANALYTICAL SYMPOSIUM & EXPOSITION 2024 Abstract Book

Eastern Analytical Symposium 2024 — Cross‑cutting advances in analytical science: concise expert summary

Significance of the topic

The 2024 EAS abstracts present a broad snapshot of contemporary analytical chemistry challenges and solutions spanning sustainability, life sciences, environmental monitoring, separations science, vibrational and mass spectroscopies, and forensic/field analysis. Advances reported address real‑world needs: greener laboratory practice; reliable analysis of complex biologics (peptides, oligonucleotides, ADCs, vaccines); sensitive environmental contaminant detection (PFAS, elemental impurities); extractables & leachables for medical devices and single‑use technologies; and high‑throughput, automation and ML to accelerate discovery and QC. The collection emphasizes translational impact — methods that support process development, regulatory compliance, and diagnostics while reducing time, waste and cost.

Goals and overview of the programmatic themes

The abstracts collectively aim to:

• Improve analytical sensitivity, specificity and throughput for complex matrices (biologics, tissues, environmental samples).
• Adopt sustainable analytical practices and reduce solvent/material footprints in routine laboratories.
• Advance structural elucidation (NMR, CD‑MS, X‑ray/MicroED) and orthogonal characterization workflows for challenging molecules and macromolecular assemblies.
• Develop robust strategies for extractables & leachables, PFAS detection, and elemental impurity quantitation compliant with contemporary regulatory expectations.
• Integrate automation, ambient/label‑free MS sampling, and machine learning to enable ultrahigh‑throughput screening and data‑rich imaging.

Methodology and analytical approaches reported

The volume showcases an extensive set of experimental and computational methodologies, including:

• Mass spectrometry advances: charge‑detection MS for megadalton particles (viruses, VLPs), high‑resolution LC‑MS/MS for PFAS and nitrosamines, coulometric MS for absolute peptide/protein quantitation, AEMS/DESI for ultrahigh‑throughput analysis, droplet‑APCI and FIA‑MS for rapid enzymatic screens, and O‑PTIR / photothermal‑IR imaging for sub‑micron chemical mapping.
• NMR innovations: i‑HMBC/isotope‑shift‑based strategies to unambiguously assign 2‑bond vs longer HMBC correlations for proton‑deficient molecules; automated qNMR using quantitative QM spectral analysis and qNMR platform development for novices.
• Separation science: two‑dimensional LC (2D‑LC), tandem‑column LC, SEC‑SEC online 2D with MALS/dRI for absolute MWs, novel capillary columns and superficially porous particle (SPP) chemistry for scalability, and hydrophilic/ion‑pair stationary phases optimized for oligonucleotide analysis.
• Spectroscopy & imaging: hyperspectral FTIR/Raman near‑field imaging for biomedical samples, widefield fluorescence‑detected photothermal IR, vibrational SHG/ NIR‑vSHG for interfacial vibrational information, and single molecule blinking approaches for dye identification.
• Proteomics & biomarker discovery: in‑solution and gel‑based nanoLC‑MS/MS workflows for serum and breast milk degradomics/proteomics aimed at early breast cancer biomarker discovery.
• Environmental & safety analytics: combustion ion chromatography (CIC) and TOP assays for total fluorine/PFAS mass balance, SERS for femtomolar PFAS detection, and ICP‑MS/ICP‑OES strategies for ICH Q3D/USP <232>/<233> elemental impurity testing.
• Sample preparation and process analytics: hybrid SPPS/LPPS continuous peptide manufacturing with UHPLC‑PAT, UF/DF (TFF) evaluation for extractables mitigation, SPE optimization for oligonucleotides, protein precipitation to improve PS80 assays, and VAMS dried blood microsampling validation for pediatric/PKU use.
• Automation, data and ML: automated ambient MS platforms (Echo/Acoustic ejection, DESI), machine learning for hyperspectral MSI, BBM (blink‑based multiplexing) and logistic regression for dye ID, and Bayesian hierarchical modeling to correct cross‑matrix calibration biases.

Key results and discussion — grouped highlights

1) Sustainability and laboratory practice

• Industry groups presented solvent‑saving chromatography tactics (small‑bore columns, alternative solvents, QbD) and R&D lab workflows to reduce energy, solvent and waste, and demonstrated economic benefits of greener practices.

2) Big‑mass and complex particle mass spectrometry

• CD‑MS reliably measures heterogenous megadalton assemblies (viruses, VLPs, gene‑therapy vectors), now with higher resolving power and chromatography timescale coupling to monitor assembly stoichiometry and intermediates.

3) NMR for difficult structure problems

• i‑HMBC enables sensitive detection of isotope‑shift signatures to assign two‑bond correlations and supports isotope‑shift based structure elucidation for proton‑deficient natural products at sub‑microgram scales.

4) Separations and assay robustness for biologics and oligonucleotides

• Online 2D SEC‑SEC with MALS/dRI provided broad MW coverage and absolute mass determination without calibration curves, accelerating process monitoring for protein mixtures and vaccines.
• New SPP/hybrid silica materials and passive surface treatments improve oligonucleotide HPLC/LC‑MS robustness at elevated pH and temperature, reducing metal surface adsorption and enabling reliable separations for 10−60mers.

5) High‑throughput and automated mass spectrometry

• Acoustic ejection MS (Echo) and DESI‑based automated platforms achieved sample throughputs at or below 1 s/sample for direct, label‑free assays and rapid reaction screening. These technologies showed applicability across medicinal chemistry, enzymology, and targeted bioassays.

6) Imaging, vibrational spectroscopy and microanalysis

• Hyperspectral near‑field FTIR/Raman and photothermal IR imaging enabled nanoscale chemical mapping of cells and tissues; O‑PTIR resolved chemical identity of sub‑visible particulates relevant to biopharma. NIR‑vSHG provides a single‑beam vibrational probe with advantages over mid‑IR SFG in accessibility and interpretation.

7) Environmental contaminants and PFAS

• LC‑HRMS plus TOP and CIC allowed identification of many previously unreported PFAS classes in AFFFs; non‑targeted and total‑fluorine approaches are critical for closing mass balances. SERS and sensitive LC‑MS/MS assays extended detection limits to environmentally relevant concentrations.

8) Regulatory and method lifecycle considerations

• Industry and regulators emphasized implementation of ICH Q14 and revised Q2(R2), highlighting AQbD, Method Operable Design Regions (MODR), robustness, and lifecycle strategies. Practical surveys and case studies underline both opportunities and barriers to adoption.

Practical benefits and applications

• Sustainability measures reduce solvent use and operating costs while maintaining data quality.
• CD‑MS and 2D‑LC workflows improve characterization of vaccines, VLPs and complex biologics for process optimization and QC release decisions.
• Ultrahigh‑throughput MS platforms compress analytical timelines for reaction screening and HTS hit validation, reducing experimental cycle times in discovery chemistry and biocatalysis.
• Advanced imaging and O‑PTIR enable forensic and pharmaceutical particulate identification without destructive sampling, supporting root‑cause analyses.
• Validated microsampling (VAMS) and improved sample prep increase accessibility to pediatric and longitudinal clinical studies.

Used instrumentation (selected categories reported across abstracts)

• Mass spectrometers: QTOF, Orbitrap/HRMS, triple quadrupole (QQQ), charge‑detection MS (CD‑MS), transportable MS, acoustic ejection coupled QQQ/QTOF, DESI‑MS, APCI, headspace‑MRR.
• Chromatography: UHPLC, 2D‑LC (RP, HILIC, ion‑exchange, SEC, SEC‑SEC), GC×GC, capillary LC columns, various particle technologies (SPP, MFPP, hybrid silica), ion‑pair RP for oligonucleotides.
• Nuclear magnetic resonance: conventional high‑field NMR, i‑HMBC, 1H/19F qNMR, qQMSA software pipelines.
• Vibrational & optical imaging: FTIR (ATR, external reflectance), hyperspectral FTIR/Raman, O‑PTIR, photothermal IR imaging, surface enhanced Raman (SERS), fluorescence‑detected widefield photothermal IR.
• Light scattering & detectors: MALS, dRI, ELSD, CAD.
• Elemental analysis: ICP‑MS/OES, combustion ion chromatography (CIC) for total fluorine.
• Microscopy & surface analysis: SEM‑EDS, cryo‑SEM, MicroED, single‑molecule fluorescence/FRET, AFM‑like near‑field probes.
• Sample handling/automation: Tecan/robotic ELISA automation, Echo acoustic ejectors, open‑port interfaces, automated cassette/array formats, automated headspace sampling.

Main limitations and methodological cautions discussed

• Matrix effects and plasma/protein binding limit straightforward cross‑matrix calibration; Bayesian hierarchical models can correct bias but do not fully replace matrix‑matched calibration for critical assays.
• Analytical detection limits for certain regulatory health advisory levels (especially PFAS) remain challenging; total‑fluorine methods complement targeted LC‑MS approaches.
• High throughput ambient MS can trade off chromatographic separation — careful validation and orthogonal confirmation remain necessary for definitive identity assignments.
• qNMR and automated spectral fitting require good digital spectral files and validation across instrument fields for broad adoption by novices.

Future trends and opportunities

• Wider adoption of greener workflows in forensic and routine QC labs—small bore/low solvent chromatography, solvent alternatives, and elimination of unnecessary purification steps.
• Increased routine use of CD‑MS and hybrid MS imaging for biologics/virus characterization and vaccine analytics coupled with cryo‑EM for structural validation.
• Expansion of ultrahigh‑throughput MS platforms (AEMS, DESI) integrated with automated reaction platforms and closed‑loop optimization for self‑optimizing chemical manufacturing.
• Convergence of ML/deep learning with high‑dimensional imaging (MSI, hyperspectral IR) to produce automated region/cell annotation and clinical prediction models.
• Growth of non‑targeted total fluorine and CIC approaches to complement targeted PFAS lists, enabling more comprehensive environmental mass balances.
• Broader acceptance of AQbD approaches (ICH Q14/Q2(R2)) and method lifecycle documentation, supported by integrated CDS + modeling tools for MODR and transferability.

Conclusions

The 2024 EAS abstracts illustrate a vibrant analytical community delivering practical innovations across spectroscopy, separations, mass spectrometry, imaging, and data science. Key themes are integration (orthogonal/online methods), sustainability, sensitivity for complex biologics and environmental analytes, and automation/ML to accelerate discovery and QC. Continued emphasis on method validation, regulatory alignment (ICH Q14/Q2), and cross‑disciplinary translation will be essential to move these advances into routine practice.

References (selected citations appearing in abstracts)

• Winston A., Sustainable Business went Mainstream in 2021, Harvard Business Review (Dec 2021).
• Lodge S., et al., Anal. Chem., 2021, 93, 3976–3986 — vignettes on advanced NMR suppression approaches.
• Nitschke P., et al., Anal. Chem., 2022, 94, 1333–1341.
• Fuertes‑Martín R., Correig X., Vallvé J.C., Amigó N., Life 2021, 11, 1407 — biomarkers GlycA/GlycB/SPC references.
• Krishnamurthy K., Magn. Reson. Chem., 2013, 51, 821–829 — CRAFT NMR fitting approach.