Multiresidue Pesticides Analysis in Cumin Seeds Using GCMS-TQ8040 NX

Importance of the topic

Cumin seeds are a widely used spice and traditional remedy with anti-inflammatory and immune-supporting properties. Due to their complex matrix rich in essential oils and pigments, monitoring pesticide residues at trace levels is critical for food safety and compliance with EU maximum residue limits (MRLs). Reliable analytical methods are essential to protect public health and ensure product quality.

Objectives and study overview

This study aimed to develop and validate a fast, sensitive, and robust method for the simultaneous determination of 169 pesticides in Indian-origin cumin seeds. The approach integrates QuEChERS sample preparation with ultra-fast GC-MS/MS using the Shimadzu GCMS-TQ8040 NX and Smart Pesticides Database for method optimization.

Methodology and used instrumentation

Sample preparation employed a QuEChERS extraction with acidified acetonitrile followed by cleanup using a sorbent mix of C18, graphitized carbon black (GCB), PSA and anhydrous MgSO₄. Extracts were evaporated, reconstituted in ethyl acetate, and filtered through 0.22 µm PTFE.

• GC-MS/MS system: Shimadzu GCMS-TQ8040 NX
• Auto-injector: AOC-20i + s, splitless injection (2 µL)
• Column: SH-I-Rxi-5Sil MS (30 m × 0.25 mm, 0.25 µm film)
• Oven program: 80 °C (2 min) → 180 °C at 20 °C/min → 300 °C at 5 °C/min (34 min total)
• Carrier gas: Helium, constant flow 40.4 cm/s
• MS conditions: EI source, ion source 230 °C, interface 280 °C, MRM transitions (1 target + 2 qualifiers per analyte)

Main results and discussion

Linearity was established with matrix-matched calibration (1–100 µg/L), achieving R² > 0.985 for all compounds. Recoveries at spiking levels of 10 and 20 µg/kg fell within 70–120%, with reproducibility (RSD_R) under 20% as per SANTE guidelines. Method limits of quantitation (LOQs) were set at 10 µg/kg for 157 pesticides and 20 µg/kg for 12 analytes, demonstrating reliable trace-level detection. Smart Pesticides Database significantly accelerated MRM method development and optimization.

Benefits and practical applications

The validated method offers:

• High throughput ultra-fast GC-MS/MS analysis
• Robust quantification of multi-class pesticides in a challenging spice matrix
• Compliance with regulatory requirements for residue monitoring
• Ease of method setup via database-driven MRM optimization

Future trends and potential applications

Advancements may include integration of faster chromatography techniques, automated sample preparation, expanded databases for emerging contaminants, and application to other complex food matrices. Machine learning–driven method refinement could further enhance throughput and selectivity.

Conclusion

A comprehensive, SANTE-compliant method was established for screening 169 pesticides in cumin seeds. The combination of QuEChERS extraction, Shimadzu GCMS-TQ8040 NX, and Smart Pesticides Database delivers sensitive, reproducible, and efficient multi-residue analysis suitable for routine quality control laboratories.

Reference

1. European Commission. EU-Pesticides Database, Pesticides EU-MRLs.
2. 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, 412–431 (2003).
3. European Commission SANTE. Guidance Document on Analytical Quality Control and Method Validation Procedures for Pesticide Residues in Food and Feed. SANTE/12682/2019.