Determination of Over 300 Pesticides in Cumin Powder

Importance of the Topic

Analysis of pesticide residues in spices such as cumin powder is critical for food safety and regulatory compliance. Cumin presents a complex matrix with pigments and lipids that can interfere with detection of multiple pesticide classes.

Objectives and Study Overview

This study aimed to develop and optimize a streamlined workflow for simultaneous analysis of over 300 pesticides in cumin powder. The approach combines QuEChERS EN extraction with Captiva EMR–LPD passthrough cleanup, followed by LC/MS/MS and GC/MS/MS detection.

Methodology and Instrumentation

• Sample Preparation: 2 g of cumin powder extracted with ACN (1% acetic acid) using Agilent Bond Elut QuEChERS EN salts.
• Cleanup: Passthrough cleanup using Agilent Captiva EMR–LPD cartridges to remove ~60% of matrix co-extractives.
• LC/MS/MS: Agilent 1290 Infinity LC coupled to 6490 triple quadrupole MS, ESI polarity switching, dynamic MRM.
• GC/MS/MS: Agilent 8890 GC with 7000E triple quadrupole MS, multimode inlet, mid-column backflush, dMRM acquisition.

Results and Discussion

• Matrix Removal: EMR–LPD removed ~60% of co-extractives, yielding cleaner extracts and lower background compared to dSPE methods.
• Recovery: 70–120% average recovery achieved for >95% of targets across LC and GC amenable pesticides.
• Precision: Relative standard deviations <20% for >97% of analytes at 10 and 100 ng/g spike levels.
• Matrix Effects: 60–130% signal suppression/enhancement for most LC-amenable compounds.
• Calibration: Linear dynamic range of 2.5–2,500 ng/g in matrix with R2 > 0.99 for 90.5% of targets.

Benefits and Practical Applications

• Simplified Workflow: Passthrough cleanup reduces sample transfers and processing time.
• High Throughput: Combines two detection platforms to cover 300+ pesticides efficiently.
• Regulatory Compliance: Meets SANTE guidelines for multiresidue pesticide analysis in spices.

Future Trends and Opportunities

• Automation of cleanup and detection to further increase throughput.
• Extension to other challenging matrices and emerging pesticide classes.
• Development of advanced sorbents for enhanced selectivity.
• Integration with high-resolution MS for accurate compound identification.

Conclusion

The proposed QuEChERS EN extraction paired with Captiva EMR–LPD cleanup and dual LC/MS/MS and GC/MS/MS analysis offers an effective, robust, and regulatory-compliant method for quantifying over 300 pesticides in cumin powder, achieving high recoveries, precision, and clean extracts.

References

• SANTE/11312/2021: EU Guidance on Analytical Quality Control and Method Validation for Pesticide Residues.
• Lacina et al. J. Chromatogr. A 2012, 1262, 8–18.
• Parmar et al. J. Sci. Food Agric. 2022, 102, 1782–1811.
• Zhao & Andrianova, Agilent Application Note 5994-5630EN, 2023.
• Zhao & Andrianova, Agilent Application Note 5994-5671EN, 2023.
• Andrianova & Zhao, Agilent Application Note 5994-4965EN, 2022.
• Zhao, Agilent Application Note 5994-4767EN, 2022.
• Agilent Technologies Inc. Determination of Over 300 Pesticides in Cumin Powder, 2023.