The manual d-SPE step in QuEChERS workflows can be a bottleneck. Learn how the PAL System automates µSPE cleanup, offering a faster, cleaner, and greener solution for food safety, environmental analysis, and beyond.
Reach out and set it up with our Swiss partners from Brechbühler.
The QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method is a cornerstone in analytical laboratories for pesticide residue analysis. While the extraction is efficient, the traditional cleanup step, known as dispersive Solid Phase Extraction (d-SPE), often remains a manual, time-consuming process. PAL System is proud to collaborate with our trusted Swiss partner, Brechbühler AG, to bring advanced automated sample preparation solutions to local laboratories.
One of the most impactful of these is the automation of µSPE for QuEChERS extracts, representing a significant step forward in lab automation and efficiency.
The Challenge with Traditional d-SPE Cleanup
The standard d-SPE step involves adding a sorbent powder directly to the sample extract to bind and remove matrix components like fats, sugars, and pigments. While effective to a degree, this manual process has several limitations:
Limited Selectivity: The cleanup is often not exhaustive, leaving behind matrix components that can contaminate the GC-MS or LC-MS system.
Manual Labor: The process is repetitive and operator-dependent, introducing potential variability and consuming valuable analyst time.
Lack of Traceability: Manual steps are difficult to track precisely, which can be a challenge in regulated environments.
This is where automation and miniaturization offer a clear advantage.
Micro Solid Phase Extraction (µSPE) replaces the manual d-SPE step with a miniaturized, cartridge-based SPE cleanup that is fully automated on the PAL RTC.
A key strength of µSPE is its versatility, allowing for two primary modes of operation depending on the analytical goal:
Pass-Through Mode (Cleanup): For applications like QuEChERS cleanup, µSPE operates in a "pass-through mode". Think of it like a highly efficient filter: the sorbent acts as a scavenger, trapping and removing unwanted matrix components while letting the valuable target analytes pass through for analysis.
Bind-Elute Mode (Enrichment): Alternatively, µSPE can be used in a "bind-elute mode". In this workflow, the sorbent is chosen to selectively bind and concentrate the target analytes from the sample matrix. Interferences are washed away, and the purified analytes are then eluted. This is ideal for trace-level analysis of specific compounds. For example, a strong anion exchange (SAX) cartridge can capture highly polar pesticides like glyphosate. Similarly, a weak anion exchange (WAX) sorbent is well-suited for retaining per- and polyfluoroalkyl substances (PFAS), a critical application in environmental monitoring.
Regardless of the mode, this automated approach offers significant benefits:
Superior Cleanup 🧼: The packed sorbent bed in the µSPE cartridge provides a much more efficient and selective cleanup than loose d-SPE powder. This leads to cleaner extracts, which significantly increases instrument uptime and ruggedness.
Full Automation 🤖: The PAL RTC automates the entire process - from conditioning the cartridge to loading the sample and eluting the cleaned extract - in as little as 8 minutes per sample. With "prep-ahead" scheduling, the PAL System prepares the next sample while the current one is running on the GC-MS, maximizing throughput.
Green Analytical Chemistry 🌱: The miniaturized format drastically reduces solvent and sorbent consumption, aligning perfectly with the principles of Green Analytical Chemistry (GAC).
Enhanced Precision & Traceability 📊: Automation eliminates manual variability, leading to exceptional precision. Every step is digitally controlled and logged, ensuring full traceability.
Broadening Horizons: Diverse Applications for Automated µSPE
While the QuEChERS workflow is a major application, the flexibility of the PAL System with µSPE technology extends to many other analytical challenges. The core principles of selective extraction and cleanup can be applied to a wide range of compounds and matrices.
Targeted Analysis of PFAS
The analysis of per- and polyfluoroalkyl substances (PFAS) is a critical task in environmental analysis. PAL System offers a robust solution for this challenge, providing a range of PFAS-free consumables to minimize background contamination. An established workflow for seafood analysis demonstrates how a QuEChERS-style extraction can be combined with automated µSPE cleanup to achieve sensitive and reliable quantification of PFAS by LC/MS, meeting stringent regulatory requirements.
In metabolomics and lipidomics, complex samples often contain lipids in a wide dynamic range, where high-abundance species can mask the detection of low-abundance ones. Automated µSPE can be used in an "enrichment mode" for sophisticated class fractionation of lipids. For instance, a single organic extract can be automatically processed through a mixed-mode µSPE cartridge to separate it into distinct fractions, such as neutral lipids, free fatty acids, and phospholipids . This approach helps to equalize the abundance of different lipid classes, preventing detector saturation and enabling a more comprehensive analysis of the lipidome.
These examples demonstrate how the PAL System with µSPE is a versatile platform for both cleanup (scavenging) and enrichment, addressing complex sample preparation challenges across various fields of research.
Your Local Partner for Automation: Brechbühler AG
While we at PAL System provide the technology for such automation, our partners at Brechbühler AG provide the local expertise, sales, and support to bring these solutions to your laboratory in Switzerland. They are your direct contact for implementing robust, efficient, and green analytical workflows.
Connect with the Brechbühler team to discuss how automating your sample preparation with the PAL System can transform your lab's productivity.
ASMS 2025 - Streamlined Analysis of Polar and Non-Polar Metabolites in Plasma Using Automated Micro-SPE LC/MS
This poster presents two use cases for streamlined lipid profiling in plasma using automated Micro Solid Phase Extraction (μSPE). Where the workflows on NIST (SRM 1950) plasma samples was tested, with spiked internal standard (Ultimate SPLASH ONE) and optimized the extraction and elution parameters. Briefly, it focused on two cartridge sorbent types Mixed-Mode Cation Exchange (MCX) and C18 (CEC) and showcased their usage.
ASMS 2025 - Fully automated implementation of EPA Method 1633 for LC-MS/MS analysis of PFAS in environmental samples using a customized robotic autosampler
Widespread use and persistence of PFAS has led to ubiquitous detection in water, soil, air, and living organisms.
US EPA Method 1633 is intended for analysis of PFAS in aqueous, solid and tissue samples using LCMS/ MS at part-per-trillion concentrations.
This method involves significant sample preparation and purification steps prior to instrumental analysis, leading to bottlenecks in sample processing.
We have developed a fully automated, online μSPE-LC-MS/MS workflow based on a customized LC TriPlus RSH SMART Advanced system for high-throughput analysis of PFAS in environmental samples following EPA Method 1633 guidelines
Automated, Green, and Efficient A Compendium on Micromethods in Analytical Sample Preparation
Discover robust, precise, and reliable analytical methods while following the principles of Green Analytical Chemistry in various fields such as Food & Food Safety, Environmental, Clinical, Life Science, and Chemical.
This eBook explores the potential of uSPE to transform analytical workflows. It highlights the key benefits of uSPE, compares it with traditional techniques and examines its application across various industries. This resource provides a comprehensive guide for scientists and lab managers looking to optimize their sample preparation processes, achieve higher precision and embrace sustainable practices in analytical chemistry.
Advancing PFAS Analysis - Robotic Automation and Streamlined LC/MS Workflows
To support the scientific community and advance PFAS analysis we are proud to offer a webinar on this topic.
Key topics:
PFAS Fundamentals: Learn about the chemistry and significance of PFAS compounds.
Sample Preparation Challenges: Understand current hurdles, regulations and best practices in PFAS extraction and purification.
Automated LC/MS Workflows: Get an overview on automated workflows and see how PAL System integrates with LC/MS to optimize sample preparation and injection.
Advantages of automated and miniaturized uSPE clean-up in pesticides residues analysis
Recent developments in pesticides analysis extend the well-established methods to higher productivity and reliability while minimizing consumption and exposition to harmful chemicals. A workflow was developed that allows automatic preparation of calibration standards, automatic sample dilution, and automatic clean-up of sample extracts on one instrument, showing that miniaturized automated solutions are reducing errors, improving analytical consistency and protecting the environment in one convenient approach.
Presented by:
Thomi Preiswerk, Senior Account Manager, CTC Analytics AG
Gwen Lim , Specialist for automated sample preparation, CTC Analytics
Ederina Ninga, Postdoc, Research Group for Analytical Food Chemistry, Danish Technical University
This application note showcases a fully automated workflow for the precise quantification of 73 PFAS in seafood. Utilizing a PAL RTC autosampler and Agilent triple quadrupole LC/MS system (LC/TQ), the method automates calibration, QuEChERS extraction, and μSPE clean-up.
See this detailed video of the uSPE workflow for the clean-up of raw pesticides extract. The PAL uSPE Cartridge is operated in scavenger mode eluting the pesticides in a clean extract. The matrix is kept on the sorbent material. The cleaned extract can be injected without waiting time online for LC/MS or GC/MS analysis. All samples are treated on the same time axis for highest reliability.
