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

Importance of the Topic

Multi residue pesticide monitoring ensures compliance with MRLs and enhances food safety. Combining UPLC and APGC on a single mass spectrometer streamlines analysis across diverse pesticide classes and reduces laboratory turnaround time.

Objectives and Study Overview

This study establishes a unified workflow for the simultaneous analysis of approximately 200 pesticide residues in fruit and vegetable samples using both UPLC MS MS and GC MS MS with atmospheric pressure GC on one tandem quadrupole instrument. Target matrices include celery, lemon, corn and kale.

Methodology and Instrumentation

Sample preparation employed a QuEChERS protocol with PSA GCB and magnesium sulfate cleanup tailored to each commodity. UPLC was conducted on an ACQUITY UPLC H Class system with a BEH C18 column and mobile phases of water and methanol both containing ten millimolar ammonium acetate. GC analysis utilized a 7890A GC equipped with an Rxi 5MS column and a CTC PAL autosampler. All analyses were performed on a Xevo TQ S micro tandem quadrupole mass spectrometer featuring a Universal Source for rapid switching between electrospray ionization in positive mode and proton transfer APGC.

Main Results and Discussion

• Linearity and Calibration Calibration curves in UPLC MS MS showed R2 greater than 0.995 for most analytes while APGC required quadratic fitting for certain compounds yet complied with regulatory guidance.
• Sensitivity Over 99 percent of pesticides were detected at 0.01 milligram per kilogram with precision below ten percent relative standard deviation for most matrices.
• Repeatability Triplicate injections yielded residuals within plus minus twenty percent and the fast scanning rate delivered a minimum of twelve data points per chromatographic peak.
• Matrix Interference RADAR full scan screening identified interferences such as tetrachlorvinphos enhancement in celery guiding decisions on additional cleanup or chromatographic adjustments.

Benefits and Practical Applications

• Single instrument configuration eliminates lengthy inlet changes and leverages a universal source to handle both liquid and gas chromatography.
• Method generation and maintenance via QuanPedia databases accelerates workflow setup and ensures version control.
• High throughput and broad analyte coverage support routine compliance testing and due diligence in the food industry.

Future Trends and Applications

Expanding the use of universal source platforms will facilitate multi ionization strategies on a single instrument. Enhanced full scan acquisition and data independent approaches will enable retrospective screening for emerging contaminants. Integration with automated data processing and expanded spectral libraries will further optimize laboratory efficiency.

Conclusion

The demonstrated multi residue method using UPLC MS MS and APGC on one tandem quadrupole mass spectrometer delivers robust high throughput analysis of pesticide residues in food matrices. It meets sensitivity and precision requirements and adheres to current regulatory guidelines while increasing operational efficiency.

Reference

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2. Kovalczuk T Jech M Poustka J Hajslova J UPLC MS MS a novel challenge in multiresidue pesticide analysis in food Analytica Chimica Acta 2006 577
3. Tienstra M Portoles T Hernandez F Mol JGJ Fast gas chromatographic residue analysis in animal feed using split injection and APGC MS MS J Chrom A 2015 1422
4. Cherta L Portoles T Beltran J Pitarch E Mol JGJ Hernandez F Application of GC MS with APGC for multiclass pesticide determination in fruits and vegetables J Chrom A 2013 1314
5. European Commission Guidance document on analytical quality control and method validation procedures for pesticide residues analysis in food and feed SANTE 11945 2015 rev 0