UPLC and APGC Multi Residue Pesticide Analysis on a Single Tandem Quadrupole Mass Spectrometer Platform

Význam tématu

The analysis of pesticide residues in fruits and vegetables at regulatory limits is critical for food safety and compliance with MRL standards. Combining UPLC and APGC on a single tandem quadrupole MS platform streamlines workflows, reduces instrument footprint, and meets the sensitivity, specificity, and throughput demands of modern analytical laboratories.

Cíle a přehled studie

This study demonstrates a unified workflow for multi-residue determination of approximately 200 pesticides in fruit and vegetable matrices at legislatively relevant levels (0.010 mg/kg). It showcases rapid inlet switching between UPLC and APGC on a single Waters Xevo TQ-S micro instrument and evaluates performance against SANTE guidelines.

Použitá metodika a instrumentace

Sample extracts were prepared by QuEChERS (AOAC 2007.01) cleanup for celery, lemon, corn, and kale. UPLC separations employed an ACQUITY BEH C18 column (1.7 µm, 2.1 × 100 mm) on an ACQUITY UPLC H-Class system. GC analyses were performed on an Agilent 7890A with a 30 m × 0.25 mm × 0.25 µm Rxi-5MS column and CTC PAL autosampler. A Xevo TQ-S micro mass spectrometer with Universal Source alternated between ESI+ and APGC ionization.

• MassLynx MS acquisition and Quanpedia database for MRM method generation
• TargetLynx XS for data processing and calibration management
• Minimal inlet-switching time (<30 min) for UPLC and APGC analyses

Hlavní výsledky a diskuse

Fast scanning speeds on the TQ-S micro provided at least 12 data points per peak even within narrow time windows (e.g., 0.006 s dwell time for 30 transitions). Over 99% of compounds were detected at 0.010 mg/kg with R^2 ≥ 0.995 (UPLC) or quadratic fits (APGC). Repeatability in four matrices yielded RSDs below 10% for >90% of analytes. Matrix-matched calibration confirmed LOQs down to 0.001 mg/kg for representative pesticides.

Přínosy a praktické využití metody

• Single-instrument platform reduces capital and maintenance costs
• High-throughput screening meets regulatory and industry surveillance needs
• Easy method updates and maintenance via Quanpedia compound database
• Sufficient sensitivity and specificity for a broad range of chemistries

Budoucí trendy a možnosti využití

• Expansion to additional analyte classes and emerging contaminants
• Further automation and integration with high-resolution MS workflows
• Development of broader compound libraries for rapid method adaptation
• Integration into routine QA/QC and regulatory monitoring programs worldwide

Závěr

The universal-source Xevo TQ-S micro platform enables robust, sensitive, and efficient multi-residue pesticide analysis by UPLC-MS/MS and APGC-MS/MS on a single instrument. The workflow meets SANTE validation criteria, simplifies method management, and supports high-throughput compliance testing at regulatory limits.

Reference

1. Shah D., McCall E., Cleland G. Single LC-MS/MS Method for Confirmation and Quantification of Over 400 Pesticides in a Complex Matrix Without Compromising Data Quality. Waters Application Note No. 720005559EN, 2016.
2. Kovalczuk T., Jech M., Poustka J., Hajslova J. UPLC-MS/MS: A Novel Challenge in Multiresidue Pesticide Analysis in Food. Analytica Chimica Acta, 577, 2006.
3. Tienstra M., Portolés T., Hernández F., Mol J. G. J. Fast Gas Chromatographic Residue Analysis in Animal Feed Using Split Injection and APGC-MS/MS. Journal of Chromatography A, 1422, 2015.
4. Cherta L., Portolés T., Beltrán J., Pitarch E., Mol J. G. J., Hernández F. Application of GC–MS/MS with Atmospheric Pressure Chemical Ionization for Multiclass Pesticides in Fruits and Vegetables. Journal of Chromatography A, 1314:224–240, 2013.
5. European Commission. SANTE/11945/2015 Guidance Document on Analytical Quality Control and Method Validation Procedures for Pesticide Residue Analysis in Food and Feed, Rev. 0, 2015.
6. AOAC. Official Method 2007.01: Pesticide Residues in Foods by Acetonitrile Extraction and Partitioning with Magnesium Sulfate, 2013.