Comparison of Different Sample Matrix Cleanup Techniques for Multiresidue Pesticide Determination in Bovine Meat Extracts

Significance of the Topic

The presence of pesticide residues in bovine meat poses a serious food safety concern due to potential impacts on human health. Effective removal of lipids and proteins from complex meat extracts is critical to ensure accurate multi-residue pesticide analysis and reliable compliance with regulatory limits.

Objectives and Study Overview

This study aimed to compare three sample cleanup techniques—Agilent Bond Elut C18, Bond Elut NH2, and Captiva EMR–Lipid cartridges—after acetonitrile-based solid–liquid extraction, evaluating their efficiency in matrix removal, pesticide recovery, and analytical performance in gas chromatography–tandem mass spectrometry analysis of 56 pesticides in bovine meat extracts.

Methodology

Samples of homogenized bovine muscle were extracted with acetonitrile to precipitate proteins and solubilize pesticides. After centrifugation, aliquots of the extract were passed through one of three cleanup cartridges. For C18 and NH2 sorbents, 4 mL of extract was directly applied. For EMR–Lipid, extracts were diluted with water (80/20 v/v) and dried over magnesium sulfate to remove residual water prior to analysis. Spiking experiments at 10, 20, and 50 µg/kg evaluated recovery and reproducibility.

Used Instrumentation

• Agilent Intuvo 9000 GC with electronic pneumatic control
• Agilent 7010B triple quadrupole GC/MS
• Agilent J&W HP-5MS Ultra Inert Intuvo column (30 m × 0.25 mm, 0.25 µm)
• Captiva EMR–Lipid, Bond Elut C18, and Bond Elut NH2 cartridges
• Ultraturrax homogenizer, vortex mixer, refrigerated centrifuge, autosampler
• MassHunter Workstation software

Main Results and Discussion

Full-scan GC/MS chromatograms revealed that C18 cleanup produced the lowest background, while NH2 showed residual cholesterol. EMR–Lipid achieved comprehensive lipid removal with minimal co-extractives. Average recoveries across 56 pesticides ranged from 62 to 119% with relative standard deviations ≤16% using EMR–Lipid. In challenging compounds (e.g., atrazine, ethoprophos), EMR–Lipid delivered recoveries between 70 and 120% and RSDs <10%, outperforming C18 and NH2.

Signal-to-noise ratios for key analytes improved markedly with EMR–Lipid (e.g., S/N up to 330 for ethoprophos and 112 for atrazine) compared to lower values with C18 and NH2, ensuring sensitive detection. Method limits of quantitation (10 µg/kg with EMR–Lipid) were below or matched maximum residue limits set by EU and Brazilian regulations for most target pesticides, whereas C18 and NH2 often exhibited higher LOQs.

Benefits and Practical Applications

• Comprehensive matrix removal reduces interference and improves sensitivity
• Consistent recoveries and precision support regulatory compliance
• Lower system maintenance and extended column lifetime
• Applicability to routine monitoring in food safety and quality control

Future Trends and Possibilities

Further developments may include automation of EMR–Lipid workflows for high-throughput screening, extension to diverse animal matrices such as poultry and fish, integration with liquid chromatography–mass spectrometry for polar analytes, and exploration of novel sorbent materials with enhanced selectivity and sustainability.

Conclusion

The EMR–Lipid cleanup method, combined with acetonitrile extraction and GC/MS/MS analysis, offers superior matrix removal, reliable pesticide recovery, and sensitive quantitation in bovine meat. It outperforms conventional C18 and NH2 sorbents and aligns with regulatory requirements, making it a robust choice for multi-residue pesticide determination.

Reference

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