Analysis of Pesticides in Foods Using a Triple Quadrupole LC/MS/MS [LCMS-8030]

Significance of the topic

Pesticide residues in agricultural produce pose significant risks to consumer health. Regulatory frameworks such as Japan’s Positive List System enforce strict limits on detectable levels of multiple pesticides. Rapid, sensitive, and reliable multi-residue analytical methods are therefore critical for food safety monitoring and quality control.

Objectives and study overview

This work aimed to develop and validate a streamlined method for simultaneous quantification of 43 representative pesticides in food matrices. Using the Shimadzu LCMS-8030 triple quadrupole mass spectrometer and a preconfigured residual pesticide LC/MS/MS method package, the study evaluated performance on mixed standards and real extracts of paprika and leek.

Methodology and instrumentation

Sample preparation followed Japan’s Ministry of Health, Labour and Welfare guidelines. Chromatographic separation was achieved on a Shim-pack XR-ODSⅡ column (75 × 2.0 mm, 2.2 µm) with a gradient of aqueous and methanolic ammonium acetate.

Instrumentation used:

• Shimadzu LCMS-8030 triple quadrupole mass spectrometer
• Electrospray ionization in positive and negative modes
• Mobile phase A: ammonium acetate in water, Mobile phase B: ammonium acetate in methanol
• Gradient: 20 % B to 95 % B over 10 min, total runtime 20 min
• Flow rate: 0.2 mL/min, injection volume: 3 µL, column temperature: 40 °C

Main results and discussion

MRM analysis of mixed standards demonstrated clear separation and excellent linearity (r2 > 0.997) over 0.5–100 ppb. All 43 compounds exhibited limits of quantification at or below 10 µg/L. In paprika and leek extracts spiked at 20 ppb, recoveries ranged from 96 % to 111 % in paprika and 70 % to 110 % in leek; lower values in leek highlighted matrix suppression effects.

Adjusting the ammonium acetate concentration in mobile phases from 5 mmol/L to 0.1 mmol/L doubled to quadrupled signal-to-noise ratios for most pesticides, further enhancing sensitivity.

Benefits and practical applications of the method

The preconfigured method package eliminates labor-intensive individual MRM optimization, allowing rapid deployment for routine monitoring. High sensitivity and short analysis time support food safety laboratories and industrial QA/QC operations in meeting regulatory demands.

Future trends and possibilities

Ongoing developments may include advanced sample cleanup to reduce matrix effects, expansion of compound panels beyond 167 substances, automation of sample preparation, and integration with high-throughput workflows. Emerging ionization sources and data-driven quantitation algorithms may further improve robustness.

Conclusion

The optimized LCMS-8030 method, combined with a residual pesticide method package, provides a robust, sensitive, and efficient solution for multi-residue pesticide analysis in food. It meets regulatory LOQ requirements and facilitates high-throughput screening in practical laboratory settings.

References

Japan Ministry of Health, Labour and Welfare Notification “Multi-residue analysis of pesticides by LC/MS – Method I”
Shimadzu residual pesticide LC/MS/MS method package documentation