Multiclass Multiresidue Analysis for Food Safety Application Workflows

Multiclass Multiresidue Analysis for Food Safety — Application Workflows Using Agilent Captiva EMR (Compendium Summary)

Significance of the topic

Multiclass multiresidue analysis addresses the routine need of food, feed, and environmental testing laboratories to detect many chemically diverse contaminants (pesticides, veterinary drugs, PFAS, mycotoxins, PAHs and other analytes) across highly variable and complex matrices. Effective sample preparation is the critical determinant of sensitivity, accuracy, precision, instrument robustness and long‑term lab throughput. The Captiva Enhanced Matrix Removal (EMR) passthrough cleanup family is presented as an alternative strategy that selectively removes matrix interferences while allowing analytes to pass, thereby improving extract cleanliness, reducing matrix effects and simplifying workflows across many matrices and regulatory contexts.

Objectives and overview of the compendium

The compendium compiles application‑driven EMR workflows developed and validated by Agilent for a wide range of target classes and matrices. Primary aims are:

• To demonstrate EMR passthrough cleanup variants (EMR–Lipid, EMR–GPF, EMR–GPD, EMR–LPD, EMR–HCF, EMR PFAS Food I/II and EMR Mycotoxins) matched to matrix types.
• To show compatibility with established extraction approaches (QuEChERS, LLE, acidified extractions) and downstream LC/MS/MS, GC/MS/MS, GC/MS and LC/HRMS workflows.
• To present performance data (recoveries, RSDs, LOQs, matrix removal, regulatory fit) across ~60+ application notes covering fresh produce, dry botanicals, oils, dairy, meats, seafood, infant foods, biosolids/soil, and cosmetics.

Methodology and sample preparation

Common methodological principles and workflow elements recurring in the compiled applications:

• Extraction: QuEChERS (EN/AOAC variants) with ACN (often acidified) or two‑step liquid‑liquid extractions (EtOAc:ACN or other solvent mixes) for fatty/dry matrices.
• Passthrough cleanup: Gravity or low‑pressure passthrough on selected Captiva EMR cartridges tuned to matrix properties: EMR–Lipid (lipid removal), EMR–GPF/GPD (general pigment removal and dry matrices), EMR–LPD (low‑pigment dry), EMR–HCF (high‑chlorophyll), EMR PFAS Food I/II (PFAS cleanup), and EMR Mycotoxins.
• Post‑treatment: Additional elution steps (e.g., organic/water mixtures), post‑drying with MgSO4 or back‑extraction into solvent compatible with GC or LC, and dilution or reconstitution for direct injection in LC methods.
• Adaptations: For PFAS, strict use of polypropylene containers, PFC‑free HPLC conversion kits and sandwiched or feed injection programs to limit contamination and maximize sensitivity.

Used Instrumentation

Representative analytical platforms and critical consumables used across applications (selected examples):

• LC/MS/MS: Agilent 1290 Infinity II/III LC systems paired with 6470/6490/6495 triple quadrupole MS; LC columns such as ZORBAX RRHD/Eclipse Plus C18 and InfinityLab Poroshell series.
• GC/MS or GC/MS/MS: Agilent 7890/8890/Intuvo GC systems with 7010/7000 series TQ detectors; J&W HP‑5ms and DB‑EUPAH columns; Ultra‑Inert liners and Intuvo guard chips.
• HRMS/TOF: Agilent Q‑TOF platforms in select matrix background comparisons.
• PFAS control: Agilent InfinityLab PFC‑free HPLC conversion kit and rigorous polypropylene consumables to reduce background contamination.
• Sample prep consumables: Agilent Bond Elut QuEChERS kits, Captiva EMR cartridges (various chemistries and sizes), EMR polish pouches (anhydrous MgSO4), Bond Elut Jr PSA where hyphenated cleanup was used.

Main results and discussion (summary of performance)

Key performance trends observed across the applications:

• Recoveries and precision: Most validated methods achieved average recoveries within typical regulatory criteria (commonly 70–120% or 60–120% depending on guideline) for the majority of analytes; RSDs were commonly < 20% and frequently < 10–15% for many matrices and analyte classes.
• Sensitivity / LOQs: LOQs met or exceeded regulatory guidance in many cases — e.g., pesticides and mycotoxins down to low ng/g, PAHs down to ~0.5–1 ng/g in infant formula and edible oils, and PFAS methods reaching ppt (µg/kg down to 0.001–0.05 µg/kg) consistent with AOAC SMPR and EPA 1633 expectations for many analytes.
• Matrix removal: EMR passthrough cleanup provided substantial reduction of co‑extractives — reported matrix‑residue removal often > 60–90% depending on cartridge/matrix, with pigment removal > 95% for leafy greens and > 90% phospholipid background reduction in dairy/cheeses.
• Robustness and uptime: Cleaner extracts translated to reduced instrument background, extended runtimes between maintenance events (demonstrated for hundreds of injections in GC or LC sequences), and improved column/liner longevity.
• Comparative advantages: EMR was frequently superior to conventional dSPE or SPE in balancing cleanup and analyte recovery, particularly for challenging lipophilic matrices (oils, nuts, fatty tissues) and pigment‑rich matrices (leafy greens, teas, spices).
• Regulatory compliance: Methods validated to SANTE guidelines for pesticides, AOAC SMPR for PFAS, and EPA Method 1633 QC guidance for PFAS tissue/soil/biosolids in many cases, showing method suitability for routine regulatory or monitoring laboratories.

Benefits and practical applications

Practical advantages and use cases highlighted by the compendium:

• Simplified workflows: Passthrough cartridges integrate readily with existing QuEChERS and LLE extraction procedures and often replace multiple dSPE steps, saving hands‑on time.
• Matrix‑adaptive cartridge selection: A small number of EMR chemistries cover broad matrix classes (lipid‑rich, pigment‑rich, dry plant material, PFAS‑sensitive), enabling a one‑size‑fits‑many approach in many laboratories.
• Reduced consumable and solvent use: Many EMR workflows eliminate additional SPE steps and reduce solvent volumes and waste, lowering operating cost and improving sustainability.
• Higher throughput and instrument uptime: Cleaner extracts reduce source contamination and carryover, enabling larger injection campaigns between maintenance cycles and more consistent quantitative performance over time.
• Regulatory readiness: Demonstrated compatibility with key regulatory test methods (EU SANTE, AOAC SMPR, EPA 1633) simplifies method adoption for compliance testing.

Future trends and opportunities

Predicted developments and practical opportunities for labs adopting EMR‑based cleanup:

• Workflow automation: Integration of EMR cartridges into automated SPE/passthrough platforms and robotic QuEChERS processing will increase throughput and reproducibility.
• Broader method consolidation: Continued expansion of validated analyte panels will allow consolidated screening methods covering hundreds of analytes across LC and GC platforms to reduce method proliferation.
• Sensitivity improvements and HRMS coupling: Wider use of high‑resolution mass spectrometry linked with cleaner EMR extracts will improve non‑target screening and retrospective data mining while maintaining low detection limits.
• Standardization and interlab studies: Wider interlaboratory validation will support standardized protocols for regulatory adoption and proficiency testing across new matrices (e.g., biosolids, cosmetics, complex processed foods).
• Sustainability and miniaturization: Development of lower‑solvent versions of EMR workflows and cartridge miniaturization to reduce waste while retaining cleanup efficiency.
• PFAS and ultra‑trace analytics: Continued refinement of PFAS‑dedicated EMR chemistries and lab consumable controls to suppress background and achieve sub‑ppt quantitation where required.

Conclusion

The Agilent Captiva EMR family provides a practical, matrix‑tailored passthrough cleanup strategy that consistently improves extract cleanliness, maintains broad analyte recoveries and reduces matrix effects across a wide range of food, feed, environmental and cosmetic matrices. The compendium demonstrates that EMR workflows can simplify sample preparation, lower operational burden, extend instrument uptime, and meet regulatory performance requirements for many multiclass multiresidue analyses. For laboratories seeking to consolidate methods and improve robustness in routine testing, EMR passthrough cleanup represents a validated, scalable option.

Reference

Selected application notes and guidance compiled in the source compendium (representative citations):

• Agilent Technologies. Multiclass Multiresidue Analysis for Food Safety: Application Workflows — Captiva EMR Application Compendium. Agilent application compendium and technical notes, 2026 (multiple application notes cited throughout, e.g., 5994‑2370EN; 5994‑4764EN; 5994‑2038EN; 5994‑7366EN; 5994‑7367EN; 5994‑8232EN; 5994‑7371EN; 5994‑7373EN; 5994‑55560EN; 5994‑1483EN; 5994‑0553EN; 5994‑7436EN; 5994‑4965EN; 5994‑6101EN; 5994‑0405EN; 5994‑8630EN).
• Agilent application notes cited by number for matrix‑specific protocols and validation: 5994‑0405EN (olive oil pesticides, EMR–Lipid), 5994‑2038EN (milk pesticides), 5994‑4764EN (berries), 5994‑4765EN (spring leaf mix), 5994‑4767EN (bell peppers), 5994‑4768EN (black pepper 510 pesticides), 5994‑5630EN (cayenne pepper), 5994‑5671EN (cinnamon), 5994‑8233EN and 5994‑1932EN (veterinary drug multi‑residue workflows), 5994‑7366EN/5994‑7367EN/5994‑7369EN/5994‑7368EN (PFAS in infant formula/baby food/produce/seafood), 5994‑7373EN and 5994‑7471EN (mycotoxins), 5994‑0553EN and 5994‑1483EN (PAHs in fish/meat/oils), 5994‑5560EN (infant formula PAHs), 5994‑2873EN (THC/CBD in chocolate).
• Regulatory and method guidance referenced across applications: SANTE 11312/2021 (pesticides), AOAC SMPR 2023.003 (PFAS), EPA Method 1633 quality control guidance (PFAS in tissue/soil/biosolids), and relevant EU regulations for PAHs.