Determination of Different Classes of Pesticide Residues in Processed Fruits and Vegetables by LC-MS Using the TSQ Quantum Ultra According to EU Directive 91/414 EEC

Importance of the Topic

Consumption of fruits and vegetables may expose consumers to pesticide residues that pose health risks. To ensure consumer safety and compliance with EU legislation on maximum residue limits for food products, sensitive and reliable methods are needed for multi residue monitoring.

Objectives and Study Overview

The study aimed to develop a multi residue liquid chromatography electrospray ionization tandem mass spectrometry method capable of detecting and quantifying 45 pesticides and their metabolites in processed fruits and vegetables according to Directive 91 414 EEC and subsequent EU regulations.

Methodology and Instrumentation

Sample preparation involved homogenization, extraction with ethyl acetate and anhydrous sodium sulfate, ultrasonic treatment, filtration, evaporation, and reconstitution in methanol followed by dilution and syringe filtration. Chromatographic separation used a C18 column on a Surveyor HPLC system with a formic acid water acetonitrile gradient. Detection employed a TSQ Quantum Ultra triple quadrupole instrument in positive electrospray mode using highly selective reaction monitoring with optimized Q1 and Q3 resolutions and dwell times.

Main Results and Discussion

The method achieved instrumental detection limits below 0.5 μg/L and linear calibration with correlation coefficients above 0.99. The H SRM mode significantly reduced matrix interference and improved signal to noise ratios, as shown in spiked pea samples. Residues of triazophos and myclobutanil were detected at levels below EU maximum residue limits.

Benefits and Practical Applications

The validated protocol provides a rapid multi residue screening tool for laboratories performing food safety and quality control analyses. It fulfills EU performance criteria and can be applied to diverse food matrices with high throughput.

Future Trends and Opportunities

Further expansion to additional pesticides and metabolites is feasible. Integration with high resolution mass spectrometry and automated sample processing may enhance sensitivity, selectivity, and throughput for emerging contaminant monitoring in food.

Conclusion

A robust LC ESI MS MS method using H SRM on a TSQ Quantum Ultra instrument enables reliable detection and quantification of low level pesticide residues in processed fruits and vegetables, ensuring compliance with EU directives.

Reference

• Directive 91 414 EEC on the placing of plant protection products on the market
• Regulation EC 396/2005 on maximum residue levels of pesticides
• European Commission SANCO 2007 3131 method validation and quality control procedures
• Botitsi E Economou A Tsipi D Multi residue analysis of pesticides by LC ESI MS MS Anal BioAnal Chem 2007 389 1685 1695