MULTIRESIDUE PESTICIDE ANALYSIS IN FRUITAND VEGETABLE COMMODITIES USING BOTH UPLC AND APGC ON A SINGLE MASS SPECTROMETER PLATFORM

Significance of Multiresidue Pesticide Analysis

Ensuring food safety requires accurate monitoring of hundreds of pesticides applied to fruit and vegetable crops. Regulatory bodies set maximum residue limits to protect consumers and enforce compliance through analytical testing. A unified workflow capable of detecting a broad range of compounds with high sensitivity and throughput is essential for both public agencies and the food industry.

Objectives and Study Overview

This study demonstrates a single mass spectrometer platform combining ultra performance liquid chromatography tandem mass spectrometry and atmospheric pressure gas chromatography tandem mass spectrometry. The goal is to analyze over 200 pesticide residues across diverse commodity classes within a rapid and reliable workflow. The method complies with SANTE 11945 2015 guidelines for sensitivity, repeatability and linearity.

Methodology and Instrumentation

Sample Preparation

• QuEChERS extraction and dispersive solid phase cleanup tailored to matrix differences in celery, lemon, corn and kale.
• Matrix matched calibration standards over 0.001 to 0.050 mg/kg with linear or quadratic fitting as appropriate.

Used Instrumentation

• Mass spectrometer Xevo TQ-S micro with Universal Source enabling rapid switching between UPLC and APGC inlets within 30 minutes.
• UPLC system ACQUITY H Class with BEH C18 column 2.1 x 100 mm, 1.7 µm; mobile phases water and methanol with 10 mM ammonium acetate; ESI positive ionization.
• GC system 7890A with Rxi-5MS column 30 m x 0.25 mm x 0.25 µm; APGC positive mode; proton transfer mechanism.

Results and Discussion

Fast scanning of the Xevo TQ-S micro ensured a minimum of 12 data points per peak even when monitoring over 400 MRM transitions. At 0.010 mg/kg spiking, more than 99% of pesticides were detected with precision better than 10 percent relative standard deviation in most cases. Many compounds remained detectable down to 0.001 mg/kg. Calibration curves yielded correlation coefficients above 0.995 for the majority of analytes and ion ratios in matrix met the 30 percent tolerance criteria.

Benefits and Practical Application

The combined platform elevates laboratory efficiency by consolidating two chromatographic techniques on a single instrument. Method setup and maintenance are streamlined through QuanPedia databases for both MS and chromatographic parameters. The approach meets global regulatory requirements while delivering high throughput and robust performance for routine surveillance and industry quality control.

Future Trends and Potential Applications

Further integration of high resolution mass analyzers may enhance selectivity for emerging contaminants. Automated sample handling and data processing powered by artificial intelligence could accelerate routine workflow. Expansion to additional commodity types and integration with non targeted screening would broaden monitoring scope.

Conclusion

A versatile, dual inlet mass spectrometry workflow has been validated for comprehensive multiresidue pesticide analysis in fruit and vegetable matrices. The method achieves regulatory sensitivity and precision while simplifying instrument utilization and method management.

Reference

1. D Shah E McCall G Cleland Single LC MS MS Method for Confirmation and Quantification of Over 400 Pesticides in a Complex Matrix Without Compromising Data Quality Waters Application Note 720005559EN January 2016
2. Kovalczuk T Jech M Poustka J Hajslova J UPLC MS MS A Novel Challenge in Multiresidue Pesticide Analysis in Food Analytica Chimica Acta 577 2006
3. Tienstra M Portoles T Hernandez F Mol G J J Fast Gas Chromatographic Residue Analysis in Animal Feed Using Split Injection and Atmospheric Pressure Chemical Ionisation Tandem Mass Spectrometry J Chrom A 1422 2015
4. Cherta L Portoles T Beltran J Pitarch E Mol G J J Hernandez F Application of Gas Chromatography Mass Spectrometry with Atmospheric Pressure Chemical Ionisation for Multiclass Pesticides in Fruits and Vegetables J Chrom A 1314 2013
5. European Commission SANTE 11945 2015 Guidance Document on Analytical Quality Control and Method Validation for Pesticide Residue Analysis in Food and Feed