Analysis of Formamidine Pesticides and Metabolites in Pork and Porcine Liver Using Agilent Captiva EMR—Lipid and LC/MS/MS

Significance of the Topic

Formamidine pesticides such as amitraz and chlordimeform are widely applied in livestock treatment. Residual traces in meat and organ tissues can impact food safety and consumer health. Reliable analysis in high fat matrices such as pork and liver supports regulatory compliance and quality control.

Objectives and Study Overview

This study aimed to develop and validate a streamlined method combining QuEChERS extraction and Agilent Captiva EMR—Lipid cleanup followed by LC/MS/MS for quantifying formamidine pesticides and their metabolites in pork and porcine liver. Key goals included achieving low limits of quantitation, high accuracy and precision, and efficient lipid removal in complex matrices.

Methodology and Instrumentation

The sample preparation workflow included:

• QuEChERS extraction with cold acetonitrile
• Cleanup using Captiva EMR—Lipid cartridges
• Matrix matched calibration and post spike quality control samples

Instrumental analysis was performed on an Agilent 1290 Infinity LC coupled to a 6495B triple quadrupole mass spectrometer equipped with Jet Stream electrospray ionization. Separation used a ZORBAX Eclipse Plus C18 column under a gradient of formic acid in water and acetonitrile. Quantitation relied on multiple reaction monitoring transitions optimized for each analyte.

Main Results and Discussion

The optimized method delivered linear calibration curves with R2 values above 0.99. Recoveries exceeded 60 percent at all spiking levels with precision RSD below 12 percent. Limits of quantitation reached 0.1 ng/g for chlordimeform and its metabolite DCDM and 0.1–1 ng/g for amitraz and 2,4 xylidine. Extraction solvent studies showed neutral acetonitrile provided the best analyte response whereas QuEChERS improved recovery of hydrophobic targets. Efficient lipid removal minimized matrix interferences.

Benefits and Practical Applications

This approach offers a fast, reliable workflow for routine monitoring of pesticide residues in high lipid food matrices. The simplified cleanup reduces solvent usage and sample handling steps while maintaining analyte integrity. Laboratories can adopt the method for regulatory compliance testing, quality assurance, and high throughput screening.

Future Trends and Possibilities

Further developments may include automation of sample preparation, expansion to additional pesticide classes and veterinary drugs, integration with high resolution mass spectrometry for non targeted screening, and application of greener solvents and sorbents for sustainable workflows.

Conclusion

A robust and sensitive method using QuEChERS extraction, Captiva EMR—Lipid cleanup and LC/MS/MS has been established for trace analysis of formamidine pesticides in pork and porcine liver. The validated procedure meets stringent performance criteria and supports food safety monitoring programs.

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