A New Standard in Analytical Workfow Design

Význam tématu

A fully integrated supercritical fluid extraction–supercritical fluid chromatography–mass spectrometry (SFE–SFC–MS) workflow addresses the growing demand for rapid, reproducible, and environmentally friendly sample analysis. By eliminating manual offline steps and harnessing the unique properties of supercritical CO2, this approach reduces preparation time, lowers solvent consumption, and enhances throughput across diverse matrices in pharmaceutical, environmental, food, and industrial applications.

Cíle a přehled studie

The study presents the Nexera UC system as a new standard in analytical workflow design. Key objectives include:

• Automating sample extraction and analysis with minimal human intervention
• Demonstrating time savings compared to conventional methods (e.g., QuEChERS, Soxhlet)
• Validating sensitivity and reproducibility improvements via splitless BPR in MS detection
• Applying the workflow to real-world cases: coenzyme Q10 in supplements, dried blood spots, polymer additives, cleaning validation, and tablet API quantitation

Použitá instrumentace

• SFE-30A supercritical fluid extractor with up to 48-position rack changer
• CO2 pump and modifier solvent pump for co-solvent delivery
• SFC-30A system featuring column oven and low-dead-volume back pressure regulator (BPR)
• LCMS-TQ triple quadrupole mass spectrometer series (8030/8040/8050/8060)
• Make-up pump and solvent supply for optimal ionization

Použitá metodika

• Supercritical CO2 extraction at 31.1 °C and 1,070 psi with 5 % methanol co-solvent
• Inline transfer of extracts to the SFC column without manual intervention
• Splitless injection via low-dead-volume BPR for up to fivefold sensitivity gain
• Automated sequence of up to 48 samples with extraction times as short as 7 min

Hlavní výsledky a diskuse

The integrated workflow yielded the following outcomes:

• Sensitivity: Splitless BPR increased signal intensity by approximately five times compared to split injection in reserpine assays.
• Time savings: Automated SFE eliminated roughly 30 min of manual prep per sample versus QuEChERS.
• Stability: Coenzyme Q10 extracted by SFE showed no oxidation, unlike traditional solvent sonication.
• Versatility: Direct DBS extraction facilitated rapid phospholipid biomarker analysis at the 1 ppm level.
• Efficiency: Polymer additive Irganox 1010 was fully extracted in 7 min rather than 10–20 h by Soxhlet.
• Cleaning validation: Swabbed detergent residues were quantified directly from the extraction vessel.
• Pharmaceutical assay: Recovery of a skeletal muscle relaxant API from tablets ranged from 98 % to 105 %.

Přínosy a praktické využití metody

The system offers significant advantages:

• Reduced operator workload and improved lab throughput
• Lower solvent usage and waste generation in line with green chemistry principles
• Enhanced reproducibility and sensitivity for trace-level analytes
• Broad applicability across sample types: solids, liquids, biological matrices, and polymers

Budoucí trendy a možnosti využití

Anticipated developments include:

• Integration with high-resolution MS for untargeted screening
• Miniaturization and micro-SFE platforms for high-throughput toxicology and metabolomics
• Further automation in regulatory and QA/QC workflows
• Expanded use of alternative co-solvents and additives for challenging analytes

Závěr

The Nexera UC platform demonstrates a paradigm shift in analytical workflows by fully automating SFE–SFC–MS processes. The approach delivers faster turnaround, greener operation, and higher sensitivity across multiple application domains.

Reference

• Hedgepeth W., Tanaka K., A New Standard in Analytical Workflow Design, Shimadzu Application Note, March 2016.