Multiclass Multiresidue Analysis for Food Safety Application Workflows

Importance of the topic

Multiclass multiresidue monitoring in food, feed, and related matrices is critical for consumer safety and regulatory compliance. Laboratories face the dual challenge of quantifying chemically diverse analytes at trace levels while removing complex matrix interferences that compromise accuracy, precision, instrument uptime, and method robustness. Enhanced Matrix Removal (EMR) passthrough cartridges provide a selective cleanup strategy that removes matrix components (lipids, pigments, phospholipids) while allowing target analytes to pass through, enabling reproducible, high‑throughput workflows compatible with QuEChERS and liquid–liquid extraction (LLE) approaches.

Objectives and overview of the compendium

This application compendium documents Agilent workflows that combine QuEChERS or LLE extractions with Captiva EMR passthrough cleanups for multiple analyte classes: pesticides, veterinary drugs, PFAS, mycotoxins, PAHs and other hydrophobic contaminants. The goals are to demonstrate: improved matrix removal, maintained or enhanced analyte recovery, compliance with regulatory/consensus guidelines (SANTE, AOAC SMPR, EPA Method 1633, national standards), and practical gains in throughput and instrument longevity across diverse matrices (fresh produce, oils, dairy, meats, dry botanicals, cosmetics, biosolids, soils, and more). The compendium summarizes 60+ application notes covering method parameters, validation outcomes, and operational highlights.

Methodology and sample preparation

• Core extraction approaches: QuEChERS (EN, AOAC, buffered/unbuffered, acidified) for most matrices; LLE (ethyl acetate/acetonitrile mixes) for fatty oils and some tissues; targeted solvent systems and acidification to stabilize analytes and limit sorbent interactions.
• EMR passthrough cleanup: cartridge formats tailored to matrix/analyte class — EMR–Lipid (regular and HF variants), EMR–LPD (low pigment dry), EMR–GPD (general pigment dry), EMR–GPF (general pigment, flow optimized), EMR–LPD, EMR–LPD/LPD-HF, EMR–Mycotoxins, and EMR PFAS Food I/II for PFAS analyses.
• Typical post‑treatment steps: additional elution (e.g., ACN:water mixtures), drying with MgSO4 polish pouches, solvent back‑extraction (isooctane) for GC analyses, dilution or reconstitution for LC/MS injection, and feed injection workflows for direct injection of EMR eluates for some PFAS assays.
• Integration with LC/MS/MS and GC/MS(/MS): methods optimized for both LC‑amenable and GC‑amenable analytes, including multisampler feed injection, hydrogen carrier with HydroInert GC sources for PAHs, and LC methods with PFC‑free HPLC conversion kits for PFAS control.

Used instrumentation

• GC platforms: Agilent 7890/8890/Intuvo series paired with 7000/7010/7010A/7010B GC/TQ or 5977/5977C MSD; specialized HydroInert sources and hydrogen carrier options used for PAHs.
• LC platforms: Agilent 1290/1260/1290 Infinity II/III with 6470/6490/6495/6475/6460/6495C triple quadrupoles and 6545 LC/Q‑TOF for high‑resolution confirmation and ruggedness testing.
• Columns: ZORBAX RRHD/Eclipse Plus C18, InfinityLab Poroshell 120 EC‑C18, and other UHPLC columns (2.1–3.0 mm dimensions, sub‑2 µm or 2.7 µm phases).
• Critical consumables: Captiva EMR cartridges (EMR–Lipid variants, EMR–GPD/GPF/GPD, EMR–Mycotoxins, EMR PFAS Food I/II), QuEChERS extraction kits (EN 15662, AOAC, veterinary drug variants), Bond Elut polish pouches (anhydrous MgSO4), and PP sample containers to mitigate PFAS contamination.

Main results and discussion

• General performance: Across many matrices, EMR workflows delivered high matrix removal (commonly >60–90% by residue weight or background scans) and produced colorless/low‑UV absorbing extracts for pigment‑rich samples.
• Recoveries and precision: Typical validated recoveries: 70–120% for the majority of pesticides, veterinary drugs and PFAS core compounds; many applications reported >90% of targets within 60–120% recovery and RSDs frequently <15% (often <10% for well‑behaved matrices). Mycotoxins and PAHs similarly met target recoveries and RSD acceptance windows for regulatory methods.
• Limits of quantitation: LOQs ranged by analyte and matrix — pesticides: sub‑ng/g to low ng/g; PFAS: meeting AOAC SMPR criteria in many matrices (LOQs down to 0.001–0.01 µg/kg for some matrices); PAHs: LOQs at or below 0.5–1 ng/g in infant formula and oils per EU limits; veterinary drugs and mycotoxins often achieved sub‑µg/kg LOQs aligned with regulatory thresholds.
• Regulatory conformance and ruggedness: Multiple methods validated against SANTE, AOAC SMPR, EPA 1633 guidance or national standards. Examples include PFAS methods that matched or improved on EPA 1633 MDLs/LOQs, and pesticide/mycotoxin methods showing excellent linearity (R2 > 0.99) and sustained instrument performance over hundreds of injections (e.g., >800 injections in a tea pesticide study with stable responses).
• Comparative advantages: EMR passthrough cleanup frequently outperformed traditional dSPE and SPE approaches for pigment removal, lipid elimination, reduced matrix effects, simpler workflows, and extended column/ion source life. Time and solvent savings were noted versus conventional SPE procedures, especially for PFAS in solids and tissues.

Benefits and practical applications

• Cleaner extracts: Reduced pigments, lipids, and phospholipids leading to improved quantitation and fewer matrix artifacts in MS and GC traces.
• Improved throughput and robustness: Passthrough cartridges simplify workflows (single‑pass cleanup), reduce hands‑on time, and lower solvent/consumable use compared to multi‑step SPE; demonstrated reductions in sample prep time (often >50% vs SPE) in PFAS and tissue workflows.
• Instrument and lab economy: Lower maintenance frequency, extended column and source lifetimes, fewer re‑runs, and consistent performance across large analyte lists improve lab productivity and operating costs.
• Method portability: Workflows were shown across a broad range of sample types — fresh produce, spices, oils, dairy, meat/tissue, feeds, biosolids, soils, cosmetics — illustrating a one‑size‑fits‑many approach by selecting appropriate EMR cartridge chemistry and bed mass.

Future trends and possibilities for use

• Wider adoption of passthrough EMR as a standard front‑end for multiclass residue analysis, enabling harmonized methods across laboratories and regulators.
• Integration with high‑throughput autosamplers and feed injection schemes (already used for PFAS and some LC workflows) to further reduce turnaround time.
• Expansion to emerging contaminants and hybrid methods that combine targeted and non‑targeted screening (LC/Q‑TOF) supported by cleaner extracts.
• Method standardization and validation across regulatory frameworks (SANTE, AOAC, EPA) to support routine deployment for compliance testing.
• Sustainability focus: reduced solvent and consumable use compared to traditional SPE, and optimization of cartridge sizes/bed masses for minimal waste without performance loss.

Conclusion

The compendium demonstrates that Captiva EMR passthrough cleanups, paired with QuEChERS or tailored extraction strategies, offer robust, reproducible, and scalable sample preparation solutions for multiclass multiresidue analysis across diverse food and environmental matrices. EMR workflows improve matrix removal, maintain or improve analyte recovery and precision, reduce instrument burden, and shorten turnaround times—making them a practical choice for modern food safety and environmental testing laboratories seeking regulatory compliance and operational efficiency.

References

• Agilent application notes and method highlights summarized in the compendium (selected IDs): Pesticides and matrices: 5994-2370EN, 5994-4764EN, 5994-4765EN, 5994-4767EN, 5994-0405EN, 5994-2038EN, 5994-1717EN, 5994-5061EN, 5994-4768EN, 5994-5129EN, 5994-5630EN, 5994-5671EN, 5994-5777EN, 5994-7436EN, 5994-7361EN.
• Veterinary drugs and organ matrices: 5994-8233EN, 5994-1932EN, 5994-7372EN, 5991-8598EN, 5994-3124EN, 5994-3680EN, 5994-1124EN, 5994-2007EN.
• PFAS workflows and EPA/AOAC validations: 5994-7366EN, 5994-7367EN, 5994-7369EN, 5994-7368EN, 5994-7370EN, 5994-7371EN, 5994-8610EN, 5994-8813EN, 5994-8232EN, 5994-8777EN, 5994-8778EN, 5994-9111EN.
• Mycotoxins: 5994-7373EN, 5994-7471EN, 5991-8694EN, 5994-0365EN, 5994-0366EN.
• PAHs and other applications: 5994-0553EN, 5994-1483EN, 5994-5560EN, 5994-2873EN, 5994-1611EN.
• Captiva EMR Reference Guide and product-specific documentation (technical companion to the application compendium).