Determination of Multiclass, Multiresidue Pesticides in Berries

Importance of the topic

The accurate analysis of multiple pesticide residues in berries is essential to ensure food safety and regulatory compliance. Berries contain high levels of pigments and other co-extractives that can cause ion suppression, matrix interferences, and contamination in GC/MS/MS systems. Effective cleanup workflows are therefore critical to achieve sensitive, reliable, and reproducible quantitation at regulatory levels.

Objectives and study overview

This study aimed to develop and validate a streamlined multiresidue GC/MS/MS method for 108 pesticides in blackberry, blueberry, and raspberry. The workflow combines QuEChERS EN extraction with an Agilent Captiva EMR–GPF passthrough cleanup cartridge. Key performance metrics—recovery, precision, linearity, and pigment removal—were assessed across low and high spiking levels.

Methodology and instrumentation

• Sample preparation: 10 g homogenized berry extracted with acetonitrile containing 1 % acetic acid via Agilent Bond Elut QuEChERS EN kit.
  
• Cleanup: 3 mL raw extract passed by gravity through a 3 mL Agilent Captiva EMR–GPF cartridge.
  
• Drying: Residual water removed with anhydrous MgSO₄.
  
• Analysis: Agilent 8890 GC with 7000D triple quadrupole MS in dynamic MRM mode; splitless injection with backflush.
  
• Calibration: Matrix-matched standards from LOQ to 500 ng/g with isotopically labeled internal standards.
  

Main results and discussion

• Cleanup efficiency: Over 99 % of pigments removed, yielding clear extracts and minimal UV absorbance at 450 nm.
  
• Recovery and precision: In blackberry, 84 of 108 pesticides met 70–120 % recovery and RSD < 20 % at 10 and 100 ng/g; a few sensitive analytes required elevated LOQs due to matrix effects.
  
• Comparison with dispersive SPE: Captiva EMR–GPF preserved recoveries of planar and pigment-sensitive compounds better than QuEChERS dSPE with graphitized carbon black, which showed up to 5 % failure rate.
  
• Matrix cross verification: Blackberry and raspberry achieved > 99 % pass rates for recovery, precision, and linearity; blueberry demonstrated pass rates above 90 %, remaining acceptable for routine screening.
  

Benefits and practical applications

• Simplified workflow: Eliminates multiple vortex and centrifugation steps associated with dispersive SPE.
  
• Wide applicability: Effective for pigmented fresh fruits, vegetables, and other complex plant matrices.
  
• Regulatory compliance: Meets common performance criteria for multiresidue pesticide analysis in food safety labs.
  
• Instrument reliability: Reduced matrix deposition enhances GC/MS/MS uptime and lowers maintenance.
  

Future trends and potential applications

Ongoing demands for higher throughput and broader analyte panels will drive further optimization of passthrough cleanup cartridges. Integration with automated liquid handling and expansion into LC-MS/MS applications will support comprehensive monitoring of pesticides and other contaminants across diverse food and environmental samples.

Conclusion

The combined QuEChERS EN extraction and Captiva EMR–GPF cleanup delivers a rapid, robust, and reliable GC/MS/MS method for over 100 pesticide residues in berries. It offers high recovery, excellent precision, and efficient pigment removal, outperforming traditional dispersive SPE approaches and supporting routine food safety testing.

References

1. González-Curbelo M Á Trends in Analytical Chemistry for sample cleanup. Trends Anal Chem 2015 71 169–185
2. Varela-Martínez D A Liquid-Phase Extraction Handbooks in Separation Science Elsevier 2020 Ch 14 399–437
3. Santos P J Analysis of multiresidue pesticides in salmon using Captiva EMR–Lipid with GC/MS/MS Agilent Technologies Application Note 5994-1717EN 2020
4. Zhao L Determination of 14 polycyclic aromatic hydrocarbons in edible oil Agilent Technologies Application Note 5994-1483EN 2019
5. Zhao L Multi-class multiresidue analysis of pesticides in edible oil by GC-MS/MS using enhanced matrix removal cartridges J Chrom A 2019 1584 1–12