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

Processed cereal-based foods for infants and young children require ultra-sensitive pesticide residue analysis to comply with strict EU maximum residue levels (MRLs). Rice-based baby food is widely consumed, so accurate quantification at low microgram-per-kilogram concentrations is critical for consumer safety.

Objectives and Study Overview

Develop and validate a robust GC-MS/MS method using atmospheric pressure gas chromatography (APGC) on a Xevo TQ-XS instrument to detect over 165 pesticides and metabolites in rice-based baby food at or below regulatory reporting limits.

Methodology and Instrumentation

A QuEChERS extraction and dSPE clean-up were applied to 5 g of hydrated sample using acetonitrile and citrate-buffered salts. Extracts were centrifuged, frozen, diluted with formic acid and acetonitrile, and directly injected without solvent exchange or large-volume injection techniques.
GC-MS/MS analysis employed previously established GC conditions coupled to a Xevo TQ-XS mass spectrometer with APGC 2.0, water modifier, 150 °C source, 280 °C transfer line, corona current 2.0 µA, auxiliary gas 200 L/h, and cone gas 265 L/h.

Main Results and Discussion

The method achieved instrument limits of detection typically ≤ 0.0003 mg/kg for 165 analytes; thiometon was detected at 0.005 mg/kg. Retention times were within ± 0.1 min of calibration standards, and 94 % of ion ratios met ± 30 % criteria. At spike levels of 0.0005 and 0.001 mg/kg, 90 % and 92 % of pesticides had recoveries between 70–120 %, respectively. Repeatability (RSDr) was ≤ 20 % for 96 % of compounds at 0.0005 mg/kg and 100 % at 0.001 mg/kg. Calibration residuals for 96 % of analytes were within ± 20 % and 95 % had r2 > 0.98.

Benefits and Practical Applications of the Method

This streamlined approach delivers high sensitivity and precision without additional solvent exchanges or specialized injection techniques, enabling rapid screening of baby foods for pesticide compliance in QC and regulatory laboratories.

Future Trends and Applications

Expanding the method to other food matrices and integrating enhanced ionization techniques could broaden pesticide monitoring capabilities. Coupling with automated data processing and high-throughput workflows will further improve laboratory efficiency.

Conclusion

The validated GC-MS/MS method with APGC on Xevo TQ-XS meets SANTE guidelines for over 166 pesticides in rice-based baby food, offering reliable detection at trace levels to support stringent regulatory testing.

Reference

1. Commission Directive 2006/125/EC on processed cereal-based foods and baby foods for infants and young children.
2. Commission Delegated Regulation (EU) 2021/1041 amending Regulation (EU) 2016/127 on pesticides in infant formulae.
3. EURL-CF Validation Report 31A, 2019.
4. SANTE/11313/2021 Guidance on analytical quality and method validation for pesticide residues.