Application Notebook - Solutions for Food Safety

Importance of the topic

Monitoring pesticide residues in food is critical to ensure public health and compliance with international regulations. With hundreds of active ingredients used in agriculture and increasingly stringent maximum residue limits (MRLs), laboratories require high-throughput, sensitive, and highly specific analytical methods to detect trace contaminants across diverse food matrices.

Objectives and Study Overview

This summary reviews three Shimadzu Application Notes (Nos. C135, C136 and C154) describing: the development of a comprehensive Pesticide MRM Library for LC-MS/MS method development; an expanded multi‐residue method for 646 pesticides using the LCMS-8060; and the implementation of an enhanced “MRM Spectrum Mode” to improve specificity and confidence in routine pesticide residue analysis.

Methodology and Instrumentation

Shimadzu’s solutions leverage triple‐quadrupole LC-MS/MS platforms and automated library tools to accelerate method creation and enhance compound verification:

• MRM Library (Note C135): Compilation of 766 certified reference standards with >6 000 optimized MRM transitions, collisional energies and full metadata (CAS, InChI, synonyms, web links).
• Multi‐Residue LCMS-8060 Method (Note C136): A single 10.5 min gradient method acquired 1 919 MRM transitions (3 per compound) for 646 pesticides, with 5 ms polarity switching and 30 000 u/s scan speed. Evaluated in QuEChERS extracts of mint, tomato and apple at 0.01 mg/kg.
• MRM Spectrum Mode (Note C154): Monitoring 6–10 fragment ions per target (1 291 transitions for 193 compounds) in a 15 min cycle (3 ms dwell, 5 ms polarity switch). Combines quantitation with in‐run product‐ion spectra for library searching and reduced false positives.

Main Results and Discussion

• Pesticide MRM Library accelerated method setup: users select targets and import optimized MRM lists directly into Shimadzu LabSolutions.
• Multi‐residue performance: LoD/LoQ at 0.01 mg/kg, linearity R²>0.996, repeatability <6% RSD. Matrix effects mitigated by up to 1:50 sample dilution.
• MRM Spectrum Mode enhanced specificity without loss of sensitivity. Comparison with conventional 2‐MRM methods showed equivalent quantitation (peak areas within 3% correlation) and improved discrimination against isobaric interferences.
• Library searching of in‐run MRM spectra provided high match scores, enabling automated compound confirmation across diverse commodities.

Benefits and Practical Applications

• Rapid method development and expansion – new target lists built in minutes.
• High throughput – 646 residues in ~10 min and 193 residues with full spectral confirmation in 15 min.
• Regulatory compliance – supports EU SANTE identification criteria and US/EPA tolerances.
• Reduced false reporting – multi‐ion confirmation and library matching improve data quality.
• Versatile matrices – validated across fruits, vegetables, spices and complex samples.

Future Trends and Opportunities

• Expansion of spectral libraries to cover emerging contaminants and degradation products.
• Integration of high‐resolution mass spectrometry and data‐independent acquisition for broader suspect screening.
• Automated workflows leveraging machine‐learning for real‐time quality control and anomaly detection.
• Cloud‐based sharing of MRM spectral libraries for global collaboration among laboratories.

Conclusion

Shimadzu’s Pesticide MRM Library, high‐speed LCMS-8060 methods and MRM Spectrum Mode together provide a powerful toolkit for efficient, sensitive and highly specific pesticide residue analysis. These solutions enable rapid method development, high throughput screening of hundreds of analytes, and robust compound confirmation to meet the demands of modern food safety laboratories.

Used Instrumentation

• Shimadzu LCMS-8050 and LCMS-8060 Triple Quadrupole MS
• Nexera UHPLC and Nexera UC Online SFE-SFC-MS Systems
• Nexis GC-2030 with FPD-2030
• Prominence-i HPLC with RF-20AXS FLD and PDA Detectors
• LabSolutions Insight Software for MRM Spectrum Library Searching

References

• Baker D.R., Barnes A., Loftus N. Shimadzu Pesticide MRM Library Support for LC/MS/MS. Application News No. C135, Shimadzu Corporation, UK, Nov. 2017.
• Baker D.R., Fages L., Capodanno E., Loftus N. Expanding Capabilities in Multi‐Residue Pesticide Analysis Using The LCMS-8060. Application News No. C136, Shimadzu Corporation, UK & Phytocontrol, France, Jun. 2016.
• Baker D.R., Titman C., Horner J., Loftus N. Applying ‘MRM Spectrum Mode’ and Library Searching for Enhanced Reporting Confidence in Routine Pesticide Residue Analysis. Application News No. C154, Shimadzu Corporation, UK & Scientific Analysis Laboratories, UK.