DETERMINATION OF PESTICIDE RESIDUES IN RICE-BASED BABY FOOD USING GC-MS/MS WITH APGC™ AFTER EXTRACTION AND CLEAN UP USING QUECHERS

Importance of the Topic

Low levels of pesticide residues pose health risks for infants and young children consuming rice based baby food This drives the need for analytical methods capable of quantifying residues at or below regulatory thresholds established by European legislation

Study Objectives and Overview

This work demonstrates a multi residue pesticide analysis workflow combining QuEChERS extraction with GC MS MS and atmospheric pressure gas chromatography ionization to determine 166 pesticides in rice based baby food at sub microgram per kilogram levels The method is validated against SANTE performance criteria to confirm applicability for compliance monitoring

Methodology and Instrumentation Used

Samples were prepared using a standard QuEChERS protocol including hydration acetonitrile extraction salt induced phase separation and dispersive SPE cleanup Extracts were acidified diluted and directly injected into a gas chromatograph coupled to a triple quadrupole mass spectrometer equipped with an APGC source and water as a modifier Key instrumental parameters included a source temperature of 150°C transfer line at 280°C corona current at 2 μA and optimized gas flows on a Waters Xevo TQ XS system

Main Results and Discussion

The method achieved instrument limits of detection at or below 0.0003 mgkg for 165 of 166 analytes Calibration linearity showed r2 values above 0.98 for 95 percent of compounds with residuals within ±20 percent SANTE tolerance Recovery studies at spike levels of 0.0005 and 0.001 mgkg produced average recoveries between 70 and 120 percent for over 90 percent of pesticides Precision assessed as RSDr was below 20 percent for 96 percent of compounds at the lower level and for all compounds at the higher level Chromatograms demonstrated clear separation and sensitive detection of priority residues

Benefits and Practical Applications

This approach provides high sensitivity selectivity and throughput for routine screening of pesticide residues in baby food matrices Compliance with stringent EU maximum residue levels is facilitated by low detection limits and robust performance The streamlined sample preparation and direct injection support efficient use in quality control and regulatory laboratories

Future Trends and Possibilities

Ongoing advances may include automation and miniaturization of sample cleanup integration with high resolution mass spectrometry for broader analyte coverage and adoption of enhanced ionization strategies Data processing improvements and digital workflows could further boost throughput and analytical confidence in complex food matrices

Conclusion

The validated GC MS MS method using APGC ionization delivers reliable quantification of pesticide residues at trace levels in rice based baby food It meets regulatory requirements for infant food safety and offers robust sensitivity accuracy and precision for routine monitoring

Reference

• Commission Directive 2006 125 EC on processed cereal based foods and baby foods for infants and young children
• Commission Delegated Regulation EU 2021 1041 amending Regulation EU 2016 127 on pesticides in infant formula and follow on formula
• EURL CF Validation Report 31A Determination of pesticide residues in rice based babyfood by LC MS MS and GC MS MS QuEChERS method 2019
• SANTE 11313 2021 Guidance Document on Analytical Quality Control and Method Validation Procedures for Pesticides Residues Analysis in Food and Feed 2019