Sample preparation solutions

Significance of the Topic

Solid phase extraction (SPE) streamlines sample preparation for analytical methods by improving extract purity, reproducibility and sensitivity. It reduces matrix effects such as ion suppression in LC-MS and extends column and detector lifetimes, making it vital in pharmaceutical, environmental, food and biochemical analysis.

Objectives and Overview of the Study

This technical resource document from Thermo Fisher Scientific aims to guide selection and optimization of SPE cartridges and syringe filters. It reviews phase selection based on sample matrix properties, describes a general six-step SPE procedure, presents method development strategies using testosterone as an example, and outlines filter membrane choices to ensure compatibility with various solvents.

Methodology and Instrumentation Used

Instrumentation Used:

• SPE cartridges and 96-well plates (SOLA, HyperSep, Retain PEP, Retain CX/AX, Hypercarb, C18/C8, phenyl, silica, Florisil, aminopropyl, cyano, diol, SCX, SAX, WCX, WAX phases)
• Thermo Scientific Titan3 and Target2 syringe filters with membranes: PTFE, PVDF, PES, nylon, cellulose acetate, regenerated cellulose, polypropylene, glass microfiber

Methodology:

• Phase selection flow chart based on sample solubility and polarity
• Six-step SPE workflow: sample pre-treatment, conditioning, equilibration, loading, washing, elution
• Optimization via stepwise wash and elution profiling (testosterone example)
• Filter membrane compatibility charts for solvent resistance

Main Results and Discussion

• Flow chart simplifies selection of SPE sorbent by matching sample matrix and analyte properties to sorbent chemistry
• Six-step SPE procedure ensures reproducible clean extracts by controlling pH, solvent strength and flow rate
• Testosterone wash/elution profile demonstrated optimal wash at 50% methanol and elution at 90% methanol for high recovery and clean extracts
• Syringe filters with pre-filters and membrane-housing compatibility tables improve filtration consistency and prevent clogging or sample loss

Benefits and Practical Applications

• Enhanced detection sensitivity and lower limits of quantitation through analyte concentration and matrix removal
• Reduced maintenance and longer lifetimes for columns and detectors by minimizing fouling and contamination
• Versatile sample preparation across pharmaceutical, environmental, food/beverage and biochemical labs
• Reliable, reproducible protocols that streamline QA/QC workflows and method validation

Future Trends and Opportunities

• Integration of automated SPE systems with online LC-MS workflows to further reduce hands-on time and error
• Development of novel sorbents targeting emerging contaminants such as microplastics, per- and polyfluoroalkyl substances and pharmaceutical residues
• Enhanced filter designs and membranes for high-throughput bioanalysis, including phospholipid removal and low nonspecific binding
• Implementation of chemometrics and AI-driven optimization to customize SPE protocols for complex matrices

Conclusion

Thermo Fisher Scientific’s comprehensive SPE and filtration solutions provide a robust framework for achieving clean, sensitive and reproducible sample extracts. The presented guidelines on sorbent selection, workflow optimization and membrane compatibility empower analytical laboratories to tailor methods for diverse applications, reducing matrix interferences and improving overall data quality.

Reference

No explicit literature references were provided in the source document.