Fast analysis of multi-class pesticides panel in wine using single run LC-triple quadrupole mass spectrometry

Significance of the topic

Accurate detection and quantification of pesticide residues in wine is essential to ensure consumer safety and to meet stringent regulatory limits. Multi-residue analysis poses challenges due to the diversity of chemical classes, low concentration levels, and complex wine matrix. A streamlined, robust LC-MS/MS approach that can handle hundreds of targets in a single run enhances laboratory throughput and confidence in food safety monitoring.

Objectives and study overview

This study demonstrates a fully validated liquid chromatography–tandem mass spectrometry (LC-MS/MS) workflow capable of quantifying over 400 pesticides in wine below their respective maximum residue limits (MRLs). The method was tested against EU SANTE/11813/2017 guidelines for accuracy, precision, sensitivity, and robustness, using both red and white wine samples.

Methodology

Sample preparation follows a QuEChERS protocol: 10 mL of wine is extracted with 10 mL acetonitrile, salts are added to induce phase separation, and the mixture is centrifuged. The supernatant is filtered via a 0.45 µm syringe filter and transferred to vials. Matrix-matched calibration standards (MMS) and matrix-extracted spikes (MES) cover concentration levels from 0.5 µg/kg to 100 µg/kg.

Instrumentation

• Thermo Scientific Vanquish Flex Binary UHPLC system
• Thermo Scientific Accucore aQ C18 Polar End-capped LC column (100 × 2.1 mm, 2.6 μm)
• Thermo Scientific TSQ Quantis triple quadrupole mass spectrometer with heated electrospray ionization (HESI)
• Thermo Scientific TraceFinder software for automated SRM data processing

Main results and discussion

Calibration curves for more than 95% of compounds exhibited correlation coefficients (r2) ≥ 0.990 over 0.5–100 ppb. MES recoveries at the LOQ met EU criteria (70–120%). Timed-SRM transitions in both positive and negative modes provided confident identification and quantification. Chromatographic run time was 15 minutes with polarity switching, ensuring ≥ 10 scans across each peak. System robustness was confirmed over 300+ injections without performance loss.

Benefits and practical applications

The workflow delivers rapid, high-throughput multi-residue analysis with minimal cleanup and small injection volume (1 μL). It meets EU regulatory requirements for pesticide monitoring in wine and can be readily adopted in routine quality control, research laboratories, and contract testing services.

Future trends and possibilities

Emerging trends include expansion of target lists to cover new pesticides and metabolites, integration of high-resolution mass spectrometry for non-target screening, and further automation of sample preparation and data review using machine learning. Miniaturized extraction techniques and multiplexed UHPLC systems may further increase sample throughput.

Conclusion

This application note outlines a comprehensive LC-MS/MS approach for simultaneous quantification of over 400 pesticides in wine. The method is fast, sensitive, and robust, aligning with EU SANTE guidelines. It supports reliable compliance testing and enhances confidence in product safety.

Reference

1. SANTE/11813/2017. Guidance document on analytical quality control and method validation procedures for pesticide residues analysis in food and feed.