Multi-Residue Pesticide Analysis in Cumin using GC-MS/MS

Importance of the Topic

Cumin (Cuminum cyminum) seeds are valued spices with long-standing medicinal uses. However, intensive cultivation often involves pesticide applications that may leave residues exceeding safety limits. Monitoring these residues is essential to ensure compliance with European Union MRLs and to protect consumer health.

Objectives and Study Overview

This study aimed to develop and validate a multi-residue GC-MS/MS method for the analysis of 169 pesticides in Indian-origin cumin seeds. A modified QuEChERS extraction was combined with Shimadzu GCMS-TQ8040 NX detection to achieve rapid, sensitive quantification.

Methodology and Instrumentation

• Sample Preparation: Ground cumin seeds underwent modified QuEChERS extraction using acetonitrile and magnesium sulfate, followed by cleanup with C18, graphitized carbon black, and PSA, then filtration through a 0.22 μm PTFE filter.
• Chromatographic Conditions: Separation on a SH-I-Rxi-5Sil MS column (30 m × 0.25 mm I.D., 0.25 μm film) with an oven program from 80 °C (2 min) to 180 °C at 20 °C/min, then to 300 °C at 5 °C/min over 34 min; helium carrier gas, splitless injection of 2 μL.
• Mass Spectrometry: Triple quadrupole MS in EI mode using one quantifier and two qualifier MRM transitions per analyte. Method setup and data processing were streamlined with Smart Pesticides Database Ver.2 and LabSolutions Insight.

Main Results and Discussion

Linearity across 1–100 µg/L showed 80–120% accuracy. Recoveries at 10 and 20 µg/kg spiking levels ranged from 70 to 120%, with reproducibility (RSD) <20%. LOQs of 10 µg/kg were achieved for 131 pesticides and 20 µg/kg for 38 compounds, meeting SANTE guideline requirements.

Benefits and Practical Applications

The validated GC-MS/MS method offers high sensitivity and throughput for routine quality control and regulatory monitoring of pesticide residues in complex matrices like cumin seeds. Its robustness supports compliance with international food safety standards.

Future Trends and Potential Applications

Advancements may include coupling with high-resolution mass spectrometry for non-target screening, expanding pesticide libraries, automating QuEChERS workflows, and developing portable instrumentation for on-site residue analysis.

Conclusion

A simple, rapid, and sensitive GC-MS/MS protocol with modified QuEChERS extraction has been established for reliable quantification of 169 pesticide residues in cumin seeds, aligning with EU MRLs and SANTE validation criteria.

References

• GB 2763-2019 National Food Safety Standard—Maximum Residue Limits for Pesticides in Food, Code of China.
• Anastassiades M., Lehotay S.J., Štajnbaher D., Schenck F.J., Fast and Easy Multiresidue Method Employing Acetonitrile Extraction/Partitioning and Dispersive Solid-Phase Extraction for the Determination of Pesticide Residues in Produce, J. AOAC Int., 86 (2003) 412–431.
• European Commission SANTE/12682/2019 Guidance Document on Analytical Quality Control and Method Validation Procedures for Pesticide Residue Analysis in Food and Feed.