Determination of Mycotoxins and Pesticides in Olives

Significance of the topic

Olive products are rich in health-promoting compounds but are vulnerable to contamination by pesticides and mycotoxins. Reliable analytical methods for simultaneous quantification of these residues are essential for food safety, regulatory compliance, and consumer protection.

Objectives and study overview

This study aimed to develop and validate a rapid, sensitive LC/MS/MS method for concurrent determination of 71 pesticides and six mycotoxins in olives. The approach combined QuEChERS extraction with Agilent Captiva EMR–Lipid cleanup and analysis on an Agilent 1260 Infinity II Prime LC coupled to an Ultivo triple quadrupole mass spectrometer.

Methodology and instrumentation

The optimized workflow used 10 g olive sample spiked with internal standards, extracted with 1% acetic acid in acetonitrile and AOAC QuEChERS salts, then frozen in liquid nitrogen for 90 s to precipitate lipids. Cleanup was performed on a 3 mL Captiva EMR–Lipid cartridge. Chromatography employed an InfinityLab Poroshell 120 SB-C18 column (2.1 × 100 mm, 2.7 µm) at 45 °C with a gradient of 0.1% formic acid in water and acetonitrile. MS detection used dynamic MRM in positive mode with an Agilent Jet Stream source.

Main results and discussion

The method achieved limits of quantification of 10 ng/g for pesticides and 2 ng/g for major aflatoxins, meeting or exceeding EU maximum residue limits. Recoveries ranged from 70% to 120% with RSDs below 20% across four concentration levels. Matrix effects were controlled through the EMR–Lipid cleanup and freeze-out step. A 14-min run time enabled high throughput while maintaining robust performance for polar and nonpolar analytes.

Benefits and practical applications

• Simultaneous multi-residue analysis streamlines laboratory workflows.
• High sensitivity and precision support compliance with EU and Brazilian MRL regulations.
• Efficient lipid removal minimizes matrix interferences, improving data quality.
• Method is adaptable for routine screening in food safety and QA/QC laboratories.

Future trends and applications

Advances in sample preparation, such as automation of EMR-Lipid cleanup, and further miniaturization of LC/MS platforms will enhance throughput and reduce solvent consumption. Integration with high-resolution mass spectrometry and data processing algorithms may expand target lists and enable non-target screening for emerging contaminants.

Conclusion

The validated Agilent Ultivo LC/MS/MS method, coupled with QuEChERS extraction and Captiva EMR–Lipid cleanup, offers a rapid, reliable solution for monitoring pesticides and mycotoxins in olives. It meets regulatory requirements and supports comprehensive food safety testing.

References

• Bucciantini M. et al. Olive Polyphenols: Antioxidant and Anti-Inflammatory Properties. Antioxidants 2021;10(7):1044.
• Hakme E. et al. Analysis of Pesticide Residues in Olive Oil and Other Vegetable Oils. Trends Anal Chem 2018;100:167–179.
• Agripoulou S. et al. Advances in Occurrence, Importance, and Mycotoxin Control Strategies in Foods. Foods 2020;9(2):137.
• Shavakhi F. et al. A Global Systematic Review and Meta-Analysis on Prevalence of Aflatoxin B1 Contamination in Olive Oil. J Food Sci Technol 2023;60:1255–1264.
• Amvrazi EG, Albanis TA. Multiclass Pesticide Determination in Olives and Their Processing Factors in Olive Oil. J Agric Food Chem 2008;56:5700–5709.
• European Commission DG-SANTE. Guidance Document on Analytical Quality Control and Method Validation Procedures for Pesticide Residues Analysis in Food and Feed, SANTE/11312/2021.
• Commission Regulation (EC) No 1881/2006. Official Journal of the European Union L 364, 2006, p 5–24.
• ANVISA. RDC No 7/2011 – Maximum Residue Limits for Pesticides in Food. Brasília: National Health Surveillance Agency.