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An Overview of Multi-residue Pesticide Testing

Others | 2022 | WatersInstrumentation
GC/MSD, GC/MS/MS, Sample Preparation, GC/QQQ, GC/API/MS, Consumables, Software, LC/MS, LC/MS/MS, LC/QQQ
Industries
Environmental, Food & Agriculture
Manufacturer
Waters

Summary

Importance of the Topic


Plant protection products are critical for global food security but can leave residues that pose health risks and trade barriers. Routine monitoring of pesticide residues in crops and foodstuffs ensures compliance with regulatory maximum residue limits (MRLs), supports due diligence in food safety, and protects consumer health and brand integrity.

Aims and Overview


This article provides a concise survey of multi-residue pesticide testing workflows. It examines regulatory drivers, key extraction and clean-up strategies, advances in chromatographic and mass spectrometric analysis, and data processing solutions designed to maximize throughput, sensitivity, and reliability.

Methodology and Instrumentation


Sample Preparation
  • Homogenization of fruits, vegetables, cereals, and animal-derived products under cold conditions to preserve labile analytes.
  • QuEChERS extraction using buffered acetonitrile to partition a broad polarity range of pesticides into an organic phase.
  • Dispersive SPE clean-up employing sorbents such as primary-secondary amine (PSA), graphitized carbon black (GCB), and C18 to remove pigments, organic acids, and lipids.
  • Alternative SPE in pass-through mode (e.g., Oasis PRiME HLB) to improve lipid removal without extensive sample handling.
  • Automation of matrix-matched standard preparation via pipetting robots to enhance precision and traceability.
Sample Analysis
  • GC-MS/MS with electron ionization (EI) and atmospheric pressure GC (APGC) soft ionization to boost molecular ion signals, improving selectivity, sensitivity, and flexibility in carrier gas choice.
  • UPLC-MS/MS employing tandem quadrupole detection in multiple reaction monitoring (MRM) for high-speed acquisition, sub-ppm sensitivity, and reduced analysis time.
  • Strategies for managing retention time requirements (minimum twice the column void volume) and ensuring stable chromatography across diverse matrices.
  • Post-injector mixing or extension loops to prevent poor peak shape of early-eluting polar analytes in high-aqueous mobile phases.
  • Assessment and compensation of matrix effects using matrix-matched calibration curves to correct for ion suppression or enhancement.
  • Data processing with exception-focused review (XFR) software modules to apply customizable quality rules for rapid, consistent evaluation of large multiresidue data sets.
Instrumentation
  • Waters ACQUITY UPLC systems and Xevo TQ Series tandem quadrupole MS (TQ-S, TQ-XS, TQ Absolute).
  • APGC source for soft ionization in GC-MS/MS.
  • Automated liquid handling platforms such as Andrew+ pipetting robot.
  • Software tools including MS Quan for MRM processing and waters_connect for data management.

Main Results and Discussion


Modern multi-residue workflows demonstrate the ability to screen hundreds of pesticides at or below global MRLs with simplified sample prep, reduced solvent usage, and higher throughput. QuEChERS combined with targeted SPE or dSPE provides clean extracts suitable for both GC and LC platforms. APGC enhances GC-MS/MS sensitivity for thermally labile or polar pesticides. UPLC-MS/MS systems deliver rapid separations with reliable quantitation even in complex matrices. Customizable data processing workflows significantly reduce manual review time and improve result consistency.

Benefits and Practical Applications


These integrated methods support regulatory compliance in food safety monitoring, enable broad-scope screening for domestic and imported commodities, and protect brand integrity. Reduced solvent costs, minimized glassware use, and streamlined workflows free resources for high-value tasks. The combined use of GC-MS/MS and LC-MS/MS covers the full spectrum of physicochemical properties of target analytes.

Future Trends and Opportunities


Ongoing innovations include further miniaturization of instruments, adoption of alternative carrier gases to address helium shortages, enhanced soft ionization techniques, and expanded automation of both sample prep and data review. Machine learning-driven peak integration and anomaly detection promise to accelerate decision making. Broadening analyte libraries and adapting workflows to new pesticide classes will maintain laboratory agility in a dynamic regulatory landscape.

Conclusion


Advancements in generic extraction (QuEChERS, SPE), sensitive tandem MS detection (GC-MS/MS with APGC, UPLC-MS/MS), and intelligent data processing form the foundation of modern multi-residue pesticide testing. These methods deliver reliable, high-throughput screening that meets stringent regulatory requirements while optimizing laboratory efficiency and reducing operational costs.

References


  • Anastassiades M et al. Fast and easy multi-residue method employing acetonitrile extraction/partitioning and dispersive solid-phase extraction for the determination of pesticide residues in produce. J AOAC Int. 86(2):412–431 (2003).
  • Lozano A et al. Miniaturisation and optimisation of the Dutch mini-Luke extraction method for implementation in the routine multi-residue analysis of pesticides in fruits and vegetables. Food Chem. 192:668–681 (2016).
  • Pihlström P et al. Analysis of pesticide residues in fruit and vegetables with ethyl acetate extraction using gas and liquid chromatography with tandem mass spectrometric detection. Anal Bioanal Chem. 389(6):1773–1789 (2007).
  • SANTE/11312/2021. Analytical Quality Control and Method Validation Procedures for Pesticide Residues Analysis in Food and Feed.

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