Comprehensive workflow for solid and semi-solid samples

Significance of the topic

Modern analytical laboratories face increasing pressure to improve throughput, reduce solvent and labor costs, and deliver trace-level, regulatory-compliant results for complex matrices (soil, food, environmental samples). Integrated, automated sample-to-report workflows that combine efficient extraction and concentration, high-performance liquid chromatography–mass spectrometry (LC–MS) analysis, and robust data processing are central to meeting regulatory requirements (e.g., PFAS analysis) and operational targets for routine and research testing. This summary reviews a comprehensive automated workflow that addresses these needs through accelerated solvent extraction, state-of-the-art LC–MS instrumentation, and an enterprise-grade chromatography data system.

Objectives and overview of the workflow

• Describe a fully integrated sample-preparation-to-report workflow for solid and semi-solid samples that minimizes manual handling and maximizes laboratory uptime.
• Present features and performance claims for automated accelerated solvent extraction and concentration, high-resolution and triple-quadrupole LC–MS analysis, and centralized data review/reporting.
• Highlight practical benefits for environmental and food-safety laboratories, including PFAS analysis equivalence to regulatory methods, improved throughput, and sustainability gains.

Methodology and workflow components

The workflow is organized into three linked stages: extract and concentrate, analyze, and report.

• Extract and concentrate: Uses the EXTREVA ASE accelerated solvent extractor, which integrates gas-assisted solvent delivery, parallel extraction capability, and automated in-line concentration. The design emphasizes reduced PFAS background, reduced solvent usage, and walk-away automation for unattended processing of multiple samples in parallel or serial modes.
• Analyze: Uses Vanquish HPLC/UHPLC systems coupled to either high-resolution Orbitrap Exploris mass spectrometers (LC-HRMS) for screening and accurate-mass analyses or TSQ Plus triple-quadrupole systems (LC–MS/MS) for targeted quantitation and SRM workflows.
• Report: Chromeleon Chromatography Data System (CDS) manages instrument control, acquisition, data processing, system suitability testing, sequence management, result reporting, and compliance features (e.g., user permissions and 21 CFR Part 11 support). Integration with LIMS is supported for end-to-end sample tracking.

Used instrumentation

• EXTREVA ASE Accelerated Solvent Extractor — gas-assisted solvent delivery, parallel extraction, automated concentration, PFAS background reduction, 2D barcode sample tracking, AI-driven endpoint detection.
• Thermo Scientific Vanquish HPLC/UHPLC Systems — robust liquid chromatography platform for high repeatability and method transferability.
• Orbitrap Exploris Series Mass Spectrometers — high-resolution accurate-mass (HRAM) MS with resolving power up to 480,000 FWHM (m/z 200), fast polarity switching, and high acquisition speed for screening and untargeted analysis.
• TSQ Plus Series Triple Quadrupole Mass Spectrometers — optimized for SRM quantitation with automated compound optimization and curated SRM libraries.
• Chromeleon Chromatography Data System (CDS) — integrated acquisition, processing, reporting, eWorkflows, SST, IRC, and LIMS connectivity.

Main results and discussion

• Automation and throughput: The described system supports fully automated extraction and concentration of up to 16 samples with parallel extraction of multiple samples—reducing manual labor and enabling true walk-away operation. Parallel modes and multi-solvent capability enable flexible scheduling and method optimization.
• Analytical equivalence and regulatory readiness: The EXTREVA ASE design is claimed to show equivalence with EPA Method 1633A for PFAS extraction, supporting confidence for regulated environmental analyses where low-level quantitation and low background contamination are critical.
• Sensitivity and robustness: Combining Vanquish LC with either Orbitrap Exploris HRMS or TSQ triple quadrupole MS yields enhanced detector sensitivity, lower baseline noise, and improved limit-of-detection/quantitation metrics. HRMS provides high-resolution separation of analyte ions from interferences, while triple-quadrupole SRM workflows provide highly selective and sensitive quantitation.
• Method development and data quality: Dedicated software tools, curated spectral libraries (e.g., mzCloud SRM entries), automated compound optimization, and SST/IRC in Chromeleon facilitate rapid method setup, consistent sequence control, and reduced out-of-specification results.
• Sustainability: The gas-assisted extraction approach reduces solvent consumption relative to traditional techniques (Soxhlet, sonication), aligning with green-chemistry goals and lowering solvent disposal costs.
• Operational efficiency: Features such as AI-driven endpoint detection for concentration, 2D barcode sample tracking, and streamlined reporting templates reduce sample mix-ups, transcription errors, and administrative overhead.

Benefits and practical applications

• Environmental monitoring: Sensitive PFAS extraction and analysis workflows suitable for compliance testing and remediation monitoring.
• Food safety and contaminant screening: Rapid extraction and high-sensitivity LC–MS workflows for pesticide residues, contaminants, and untargeted screening campaigns.
• High-throughput QC laboratories: Automated sample handling and consolidated data systems reduce hands-on time and increase sample throughput.
• Method transfer and validation: Software-driven templates and instrument robustness support reproducible method transfer between labs and streamlined validation workflows.

Future trends and potential applications

• Greater automation and AI: Expansion of machine-vision and AI tools for smarter endpoint detection, predictive maintenance, and automated method optimization will further reduce human intervention and errors.
• Greener extraction chemistry: Continued development of solvent-minimizing extraction approaches, alternative solvents, and microextraction strategies will reduce environmental impact and cost.
• Hybrid analytical strategies: Broader adoption of HRMS screening followed by targeted triple-quadrupole confirmation will become standard for laboratories balancing discovery and routine quantitation needs.
• Cloud-enabled data workflows: Cloud or hybrid data-management, combined with LIMS connectivity and centralized spectral libraries, will accelerate collaborative method development and cross-laboratory harmonization.
• Expanded spectral libraries and automation: Larger curated SRM and HRAM libraries plus automated annotation tools will shorten the path from raw data to definitive identification and reporting.

Conclusion

The integrated sample preparation—LC–MS—data-management workflow described here addresses major laboratory pain points by combining an automated, low-solvent accelerated extraction/concentration system with high-performance LC–MS instrumentation and unified data processing. This approach improves throughput, reduces solvent use and manual errors, and supports regulatory-compliant analyses (notably PFAS). For laboratories focused on environmental, food-safety, or high-throughput QA/QC testing, the described solution provides a pragmatic path to higher productivity and reliable trace-level results while enabling future enhancements through AI, greener protocols, and enhanced data connectivity.

References

• U.S. Environmental Protection Agency. Method 1633A: PFAS in Solid Waste; EPA regulatory method referenced for PFAS extraction equivalence.
• Thermo Fisher Scientific product literature: EXTREVA ASE Accelerated Solvent Extractor; Vanquish HPLC/UHPLC Systems; Orbitrap Exploris Series; TSQ Plus Series; Chromeleon Chromatography Data System and mzCloud spectral resources.