Expanding Capabilities in Multi-Residue Pesticide Analysis Using The LCMS-8060

Significance of the topic

The reliable detection and quantification of pesticide residues in food commodities is critical to ensure consumer safety and regulatory compliance. As global population pressures drive increased agricultural output, herbicides, insecticides and fungicides are widely applied at various stages of crop production. However, residual traces of these compounds may pose health risks, leading authorities in North America, Europe and Asia to enforce maximum residue levels (MRLs), often at stringent limits around 0.01 mg/kg. This regulatory landscape demands highly sensitive, specific and efficient analytical methods capable of monitoring hundreds of pesticide targets under stringent throughput requirements.

Objectives and study overview

This application note presents the development and validation of a fast, multi-residue LC/MS/MS method for the simultaneous screening and quantitation of 646 pesticides in food matrices using the Shimadzu LCMS-8060 triple quadrupole mass spectrometer. By combining a comprehensive Pesticide MRM Library with optimized chromatography and fast polarity switching, the study aims to streamline method development, achieve broad compound coverage in a single 10.5 minute gradient, and demonstrate robust performance across different sample types.

Methodology and instrumentation used

• Sample preparation: QuEChERS extraction of mint, tomato and apple matrices to produce raw acetonitrile extracts spiked with 646 pesticides; atrazine-d5 and diuron-d6 used as internal standards.
• Liquid chromatography: Shimadzu Nexera UHPLC system equipped with a Restek Raptor Biphenyl column (2.1 mm × 100 mm, 2.7 µm), operated at 35 °C with a 0.4 mL/min binary gradient from 3 % to 100 % methanol in 2 mM ammonium formate/0.002 % formic acid over 10.5 minutes, followed by re-equilibration.
• Mass spectrometry: Shimadzu LCMS-8060 triple quadrupole with heated electrospray ionisation source; polarity switching in 5 ms; acquisition speed 30,000 u/s; interface 350 °C; heating block 300 °C; desolvation line 150 °C; optimized gas flows for heating, drying and nebuliser gases.
• MRM library: Shimadzu Pesticide MRM Library containing 766 compounds, each with multiple optimized transitions. Three MRM transitions per target pesticide were selected, yielding a total of 1,919 transitions (1,819 positive mode, 100 negative mode).
• Calibration and quantitation: Six-point calibration curves from 0.002 to 0.1 mg/kg (2–100 pg/µL), using 1/C weighting. All compounds showed linearity with R² ≥ 0.99.
• Performance evaluation: Repeatability assessed by 100 consecutive injections over 24 h and 300 injections over 72 h. Matrix dilution experiments (1:5, 1:10, 1:20, 1:50, 1:100) evaluated to mitigate ion suppression.

Main results and discussion

The optimized LCMS-8060 method quantified 646 pesticides in under 11 minutes with high data density, even resolving 25 co-eluting compounds within a 15 second window. Repeatability tests yielded RSDr values below 6 % across continuous injections, and calibration curves in mint and tomato matrices achieved R² values above 0.996 for all targets. Long-term stability over 300 injections demonstrated consistent peak areas (<6 % variance) across apple, mint and tomato extracts. Sample dilution by factors of 10–50 reduced matrix-induced ion suppression, restoring recoveries to 70–120 % with RSDr ≤ 20 %.

Benefits and practical applications

• High-throughput multi-residue screening of hundreds of pesticides in a single LC/MS/MS run enhances laboratory productivity.
• Fast polarity switching and high acquisition speed deliver sensitive quantitation at or below typical MRLs.
• Integration with a comprehensive Pesticide MRM Library simplifies method setup, transition management and reporting.
• Sample dilution strategies reduce matrix interferences without adding complex cleanup steps, increasing instrument uptime.
• Suitable for routine monitoring programs in QC laboratories, regulatory compliance testing and large-scale food safety initiatives.

Future trends and possibilities of use

Ongoing expansion of spectral libraries and emergence of new pesticide chemistries will benefit from the LCMS-8060’s high-speed acquisition and robust polarity switching. Advances in automated data processing, AI-driven peak annotation and real-time quality checks are expected to further streamline workflows. Coupling with orthogonal separation techniques or high-resolution MS could deliver even greater selectivity for complex matrices and low-level contaminants.

Conclusion

The single-run LCMS-8060 method, combined with the Shimadzu Pesticide MRM Library, provides a rapid, sensitive and robust platform for quantifying 646 pesticides across diverse food matrices. Its high throughput, excellent repeatability and straightforward workflows meet the demands of modern food safety testing and support global regulatory compliance efforts.

References

1. Commission Regulation (EC) No 396/2005 of the European Parliament and of the Council on maximum residue levels of pesticides in or on food and feed of plant and animal origin. Official Journal of the European Union L70, 2005, pp. 1–16.
2. US Environmental Protection Agency. Electronic Code of Federal Regulations, Title 40, Part 180 – Tolerances and Exemptions for Pesticide Chemical Residues in Food, 2020.
3. Japanese Ministry of Health, Labour and Welfare, Department of Food Safety. Director Notice on Analytical Methods for Residual Compositional Substances of Agricultural Chemicals, Feed Additives, and Veterinary Drugs in Food (Syoku-An No. 0124001, 24 January 2005; amendments 26 May 2006).