Analysis of Pesticide Residues in Chicken Muscle with QuEChERS and Triple Quadrupole GC

Importance of the Topic

Monitoring pesticide residues in poultry products is essential to ensure food safety, comply with regulatory maximum residue limits (MRLs), and protect public health. Rapid, reliable, and sensitive analytical methods capable of quantifying multiple pesticide classes at parts-per-billion levels are critical for quality control in food production and regulatory compliance.

Objectives and Study Overview

This study aimed to develop and validate a high-throughput GC/MS/MS method for simultaneous determination of 54 pesticides in chicken muscle using QuEChERS sample preparation. Key goals included:

• Establishing a QuEChERS AOAC-based extraction protocol with two dispersive-SPE cleanup variants.
• Implementing a triple quadrupole GC/MS in multiple reaction monitoring (MRM) mode for selective detection.
• Achieving quantification limits at or below 5 ng/g (5 ppb) despite matrix interference.
• Evaluating recoveries, reproducibility, linearity, and compliance with regulatory standards.

Methodology and Instrumentation

Sample Preparation:

• Homogenize 7.5 g chicken muscle, spike with internal standard (triphenyl phosphate) and QC solutions.
• Extract with 15 mL acetonitrile acidified with 1 % acetic acid following AOAC QuEChERS salt addition.
• Perform dispersive-SPE cleanup using two kits: one tailored for “other food methods” and one for “all food types.”
• Centrifuge, transfer supernatant, dry under nitrogen, reconstitute in 1 mL acetonitrile.

Chromatography and Detection:

• Agilent 7890A GC with HP-5ms Ultra Inert capillary column (30 m×0.25 mm, 0.25 µm film). Constant carrier flow 1.0 mL/min, temperature program from 60 °C to 310 °C.
• Agilent 7000B Triple Quadrupole GC/MS System in electron ionization (EI) mode; source at 300 °C, quadrupole at 180 °C, nitrogen collision gas.
• MRM transitions optimized for each pesticide; retention times ranged from 4.6 to 18.2 min.

Results and Discussion

Clean-up Comparison:

• Extracts cleaned with the “all food types” kit appeared clear versus slightly yellow with the “other food” kit.
• Both protocols effectively removed matrix co-extractives, as demonstrated by blank chromatograms free of interfering peaks.

Analytical Performance:

• Linearity over 5–100 ng/g with correlation coefficients (R²) between 0.996 and 0.999.
• Limits of quantification at 5 ng/g, below typical MRLs for poultry.
• Recoveries for all compounds ranged from 70 % to 120 % with relative standard deviations (RSDs) below 15 % across both cleanup methods.

Benefits and Practical Applications

This approach offers a streamlined workflow capable of quantifying a broad spectrum of organochlorine, organophosphate, and pyrethroid pesticides in high-fat matrices. It supports routine monitoring in food testing laboratories, ensuring compliance with regulations and safeguarding consumer health.

Future Trends and Applications

Advancements may include:

• Integration of high-resolution mass spectrometry (HRMS) for non-targeted screening and confirmation.
• Automation of sample preparation to increase throughput and reproducibility.
• Adoption of greener solvents and miniaturized extraction techniques to reduce solvent consumption and waste.
• Extension to other animal-derived matrices such as eggs, dairy, and fish.

Conclusion

The validated QuEChERS–GC/MS/MS method using Agilent Bond Elut extraction and cleanup kits provides rapid, sensitive, and reliable multiresidue analysis of 54 pesticides in chicken muscle. Achieving low quantification limits and acceptable validation criteria, the protocol is well suited for regulatory and quality control laboratories.

Instrumentation

• Agilent 7890A Gas Chromatograph
• Agilent 7000B Triple Quadrupole GC/MS System
• Agilent J&W HP-5ms Ultra Inert Column (30 m×0.25 mm, 0.25 µm)
• Agilent Bond Elut QuEChERS AOAC Buffered Extraction Kit
• Agilent Bond Elut QuEChERS Dispersive-SPE Kits (Other Food Methods and All Food Types)

References

• Agilent Technologies Application Note 5991-2182EN, March 2013