Automated Solutions using Smart SPE to solve challenging applications

Importance of the Topic

Automated sample preparation is a critical bottleneck in modern analytical workflows. Smart SPE (Instrument Top Sample Preparation, ITSP) integrates solid-phase extraction directly on autosamplers, improving robustness, reproducibility and throughput for demanding LC/MS and GC/MS applications across clinical, environmental and food laboratories.

Objectives and Study Overview

This work reviews several fully automated Smart SPE solutions developed by Anatune to address complex sample matrices. Key applications include: Vitamin D2/D3 quantification in human serum; metaldehyde residue analysis in water; amino acid profiling via in-line derivatisation; enrichment of trace taste and odour compounds; and on-line filtration for UHPLC.

Methodology and Instrumentation

Smart SPE uses positive-pressure control to deliver precise flow through SPE cartridges mounted on a Gerstel multipurpose sampler (MPS). General workflow:

• Condition SPE cartridge with organic solvent and water
• Load sample under controlled pressure
• Wash interferences with appropriate solvent
• Dry cartridge using inert gas (for GC/MS methods)
• Elute analytes into autosampler vial
• Transfer eluate to LC or GC inlet via switching valve or cooled injection system

Specific protocols:

• Vitamin D2/D3: Protein precipitation, centrifugation, SPE clean-up, LC/MS/MS (Agilent 6460 QQQ, APCI+)
• Metaldehyde: Headspace syringe loading, SPE on Biotage ENV cartridge, nitrogen drying, dichloromethane elution, GC–MS with cooled injection
• Amino acids: Alkyl-chloroformate derivatisation on MPS, cation-exchange SPE clean-up, vortexing, centrifugation, direct LC/MS analysis

Instrumentation Used

• Gerstel Multipurpose Sampler (MPS) 2 XL
• Anatune CF100 and CF200 robotic centrifuges
• Gerstel mVORX multi-position vortexer
• Agilent 1200 LC system
• Agilent 6460 and 6410 Triple Quadrupole mass spectrometers
• Cooled Injection System (CIS 4)
• Headspace syringes (2.5 mL, 10 µL)
• Biotage ENV SPE cartridges

Main Results and Discussion

• Vitamin D workflow processes >200 serum samples per week at Guy’s and St Thomas’; calibration curves for 25-OH-D2 and 25-OH-D3 showed R² ≥ 0.998, with excellent precision.
• Metaldehyde method at Severn Trent Water achieved a six-point calibration (R² = 0.999), LOD of 0.002 µg/L and recoveries of 94.5–99.6% at two spiking levels.
• Amino acid derivatisation SPE method delivered linear eight-point calibrations, supporting diagnostic and quality-control analyses in diverse sectors.

Benefits and Practical Applications

• High throughput and reproducibility enable hundreds of analyses per week in clinical and environmental labs.
• Positive-pressure SPE ensures consistent flow and reduces method variability.
• Versatile platform accommodates a wide range of applications, from vitamins and pesticides to metabolites and odour compounds.
• On-line filtration for UHPLC minimizes downtime due to column blockages.

Future Trends and Opportunities

Smart SPE is poised to expand into multi-dimensional workflows, on-line derivatisation, and integration with ultra-high-throughput UHPLC–MS systems. Emerging areas include trace contaminant monitoring, flavour and fragrance profiling and automated QA/QC in regulated environments.

Conclusion

Smart SPE (ITSP) provides a robust, high-throughput, and flexible sample preparation solution for both LC/MS and GC/MS workflows. Its implementation across clinical, environmental and food laboratories demonstrates significant gains in efficiency, reproducibility and analytical performance.

Reference

No formal literature references were provided in the original text.