Determination of Over 300 Pesticides in Cinnamon

Significance of the Topic

Cinnamon powder is widely used as a spice and in traditional medicine but can accumulate a broad range of pesticide residues during cultivation and processing. Reliable multiresidue analysis in such complex, pigmented matrices is essential to ensure consumer safety, regulatory compliance, and product quality.

Objectives and Study Overview

This work aimed to develop and optimize a high-throughput method for the simultaneous determination of over 300 pesticides in cinnamon powder. The approach combines Agilent Bond Elut QuEChERS AOAC extraction with Captiva EMR–GPD passthrough cleanup, followed by detection with LC/MS/MS and GC/MS/MS.

Methodology and Instrumentation

Sample preparation involves:

• Hydration of 1.5 g cinnamon powder with 4 mL water containing 0.1 % formic acid
• Extraction with ACN using Agilent QuEChERS AOAC kit
• Passthrough cleanup with Captiva EMR–GPD cartridge to remove lipids, pigments, and co-extractives

Instrumentation used:

• LC/MS/MS: Agilent 1290 Infinity LC system coupled to 6490 triple quadrupole MS with JetStream ESI
• GC/MS/MS: Agilent 8890 GC with 7000E triple quadrupole MS, multimode inlet, midcolumn backflush, and dynamic MRM acquisition

Main Results and Discussion

The optimized method achieved efficient matrix cleanup and robust quantitation:

• ~60 % reduction in co-extractive residue by weight after EMR–GPD cleanup
• Target recoveries of 70–120 % for > 95 % of over 300 pesticides at spiking levels of 10 and 100 ng/g
• Reproducibility with RSD < 20 % for > 97 % of targets
• Matrix background cleanup improved by 4–10 % compared to traditional dSPE methods
• Calibration linear dynamic range from 5 to 5 000 ng/g with R2 > 0.99 for > 88 % of targets

Optimization of water premixing (10 % v/v) before cleanup balanced recovery of sensitive pesticides and matrix removal.

Benefits and Practical Applications

This method offers a simplified, time-efficient workflow that reduces analyst effort and instrument downtime. It supports regulatory monitoring and quality assurance in food and beverage laboratories by enabling reliable screening of a large pesticide panel in challenging spice matrices.

Future Trends and Potential Applications

Further integration with automated sample processing and high-resolution mass spectrometry could enhance throughput and sensitivity. The EMR–GPD cleanup approach may be extended to other complex dry matrices, such as herbs, teas, and powdered supplements, to meet evolving regulatory requirements and safety standards.

Conclusion

The combined QuEChERS AOAC extraction and Captiva EMR–GPD cleanup method, paired with LC/MS/MS and GC/MS/MS detection, delivers reliable multiresidue analysis of over 300 pesticides in cinnamon powder. Its strong matrix removal, high recovery, and reproducibility make it a valuable tool for routine food safety testing.

References

1. European Commission. EU Pesticides Database. https://ec.europa.eu/food/plant/pesticides/eu-pesticides-database/, accessed 2023.
2. SANTE/11312/2021. Analytical quality control and method validation procedures for pesticide residues analysis in food and feed. European Commission, 2021.
3. Lacina O, et al. Critical assessment of extraction methods for simultaneous determination of pesticide residues and mycotoxins in fruits, cereals, spices and oil seeds. J Chromatogr A. 2021;1262(4):8–18.
4. Zhang Z, et al. Evaluation of cleanup procedures in pesticides multi-residue analysis with QuEChERS in cinnamon bark. Food Chem. 2019;276:140–146.
5. Andrianova A, Zhao L. Five Keys of Unlock Maximum Performance in the Analysis of Over 200 Pesticides in Challenging Food Matrices by GC/MS/MS. Agilent Technologies Application Note 5994-4965EN, 2022.
6. Zhao L, Wei T. Determination of Multiclass, Multiresidue Pesticides in Spring Leaf Mix Using Captiva EMR–HCF Passthrough Cleanup and LC/MS/MS. Agilent Technologies Application Note 5994-4765EN, 2022.
7. Zhao L, Andrianova AA. Determination of Over 300 Pesticides in Cayenne Pepper Using Captiva EMR–GPD Passthrough Cleanup and LC/MS/MS and GC/MS/MS. Agilent Technologies Application Note 5994-5630EN, 2023.