Determination of Over 300 Pesticides in Cayenne Pepper

Significance of the topic

Spices such as cayenne pepper are widely consumed for flavor and may contain pesticide residues due to agricultural treatments.
Accurate monitoring of these residues is essential to meet regulatory limits and ensure consumer safety in global markets.

Objectives and study overview

This study aimed to develop and optimize a simple and robust multiresidue method for over 300 pesticides in cayenne pepper powder.
It combines Agilent Bond Elut QuEChERS AOAC extraction with Captiva EMR–GPD pass-through cleanup, followed by LC/MS/MS and GC/MS/MS analysis.

Methodology and instrumentation

• Sample preparation used 3 g of pepper powder, extraction with acetonitrile and QuEChERS salts, followed by water premixing and Captiva EMR–GPD cleanup.
• LC/MS/MS analysis was performed on an Agilent 1290 Infinity II system coupled to a 6490 triple quadrupole mass spectrometer with ESI source.
• GC/MS/MS analysis used an Agilent 8890 GC coupled to a 7000E triple quadrupole, multimode inlet, dual 15 m columns with backflush and dynamic MRM acquisition.
• Calibration employed matrix-matched standards from 2.5 to 2 500 ng/g, with linear or quadratic regression and 1/x weighting.

Main results and discussion

• Over 92% of targets achieved recoveries between 70 and 120% at spiking levels of 5 and 50 ng/g; >97% of targets had RSD < 20%.
• Matrix removal reached approximately 60% as measured by dried residue weight, significantly reducing matrix interferences compared to dispersive SPE.
• Matrix effects were controlled by dilution and cleanup, supporting sensitive quantitation for both LC- and GC-amenable compounds.
• Matrix-matched calibration curves for 86% of compounds exhibited full dynamic range with linear regression and R² > 0.99.

Benefits and practical applications

The streamlined pass-through cleanup saves time and reduces solvent usage while delivering high throughput and reliable quantitation in challenging spice matrices.
It is suitable for routine pesticide residue testing in food safety and regulatory laboratories.

Future trends and potential applications

• Integration of automated sample handling to increase throughput and reproducibility.
• Expansion of the pesticide panel to include emerging structures and transformation products.
• Application of high-resolution mass spectrometry for non-target screening in complex matrices.
• Development of sorbents tailored for other difficult matrices such as spices, herbs, and botanical extracts.

Conclusion

The combination of QuEChERS AOAC extraction and Captiva EMR–GPD cleanup enables reliable analysis of over 300 pesticides in cayenne pepper powder by LC/MS/MS and GC/MS/MS, offering efficient matrix removal and high quantitation performance.

References

1. SANTE/11312/2021 Analytical Quality Control and Method Validation Procedures for Pesticide Residues Analysis in Food and Feed.
2. Liu X et al Determination of Pesticide Residues in Chilli and Sichuan Pepper by UPLC-QTOF-MS Food Chemistry 2022.
3. Liu Y et al Rapid Screening of 27 Pesticides in Chili Powder by UPLC-QTOF-MS Chinese Journal of Chromatography 2018.
4. Zhao L and Wei T Determination of Multiclass Multiresidue Pesticides in Spring Leaf Mix Using Captiva EMR-HCF Cleanup and LC/MS/MS Agilent Technologies 2022.
5. Andrianova A and Zhao L Five Keys to Unlock Maximum Performance in Analysis of Over 200 Pesticides by GC/MS/MS Agilent Technologies 2022.