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

Importance of the topic

Cumin is a widely used spice and medicinal seed that can accumulate pesticide residues. Monitoring these residues is essential to comply with regulatory maximum residue limits and ensure consumer safety. Accurate analysis supports food quality control and public health.

Objectives and overview of the study

This work aimed to develop and validate a multi-residue gas chromatography tandem mass spectrometry method for quantifying 169 pesticide compounds in cumin seeds. The study includes method optimization, calibration, and validation according to SANTE guidelines.

Methodology and instrumentation

Sample preparation was based on a modified QuEChERS protocol. Key steps include:

• Extraction with acetonitrile and magnesium sulfate
• Cleanup using PSA, C18, and graphitized carbon black sorbents
• Filtration through PTFE membrane

Instrument configuration:

• Shimadzu GCMS-TQ8040 NX system
• SH-I-Rxi-5Sil MS column
• Splitless injection at 250 C
• Oven temperature ramp from 80 C to 300 C over 34 minutes
• Helium as carrier gas with constant linear velocity

Matrix matched calibration standards ranged from 1 to 100 micrograms per liter.

Main results and discussion

Linearity of all target pesticides showed 80 to 120 percent accuracy across the calibration range. Limits of quantification were established at 10 micrograms per kilogram for 131 compounds and 20 micrograms per kilogram for 38 compounds. Recovery experiments at these levels yielded mean values between 70 and 120 percent. Precision tests demonstrated relative standard deviations below 20 percent, meeting SANTE criteria. A few analytes were found at trace levels in blank samples and excluded from recovery evaluation.

Benefits and practical application of the method

This validated approach is simple, sensitive, and adaptable to high-sugar matrices such as spices. It provides reliable quantification for routine testing in quality control and regulatory laboratories. High throughput and compliance with international guidelines make it suitable for large-scale residue monitoring.

Future trends and possibilities

Further developments may include application to other spice matrices, integration with high-resolution mass spectrometry, and automated data processing using advanced spectral libraries and algorithms. Emerging technologies could enhance throughput and extend the range of detectable compounds.

Conclusion

A robust GC-MS/MS method was established for the simultaneous analysis of 169 pesticides in cumin seeds. The protocol meets regulatory validation requirements, offering high sensitivity, accuracy, and reproducibility for food safety monitoring.

Reference

1. GB 2763-2019 National Food Safety Standard Maximum Residue Limits for Pesticides in Food
2. Anastassiades M, Lehotay SJ, Stajnbaher D, Schenck FJ Fast and Easy Multiresidue Method Employing Acetonitrile Extraction Partitioning and Dispersive Solid Phase Extraction for Determination of Pesticide Residues in Produce J AOAC Int 86 412 431 2003
3. SANTE Guidance document on analytical quality control and method validation procedures for pesticide residues in food and feed SANTE 12682 2019