Determination of Over 300 Pesticides in Tobacco

Importance of Topic

Tobacco is a globally consumed agricultural product requiring rigorous safety evaluation. Pesticides applied during cultivation and storage can persist in the leaf matrix, posing health risks. Reliable multiresidue methods are essential to monitor regulatory guidance residue levels (GRLs) and ensure consumer safety.

Objectives and Study Overview

This study aimed to develop and optimize a streamlined method for simultaneous analysis of over 300 pesticides in tobacco. The workflow combines Agilent Bond Elut QuEChERS EN extraction with Captiva EMR–LPD passthrough cleanup, followed by detection using LC/MS/MS and GC/MS/MS. Performance was benchmarked against traditional dispersive SPE.

Methodology

The protocol begins with grinding and hydration of tobacco leaf powder, followed by QuEChERS EN extraction in acidified acetonitrile. A portion of the crude extract is mixed with water and passed through Captiva EMR–LPD cartridges under gentle pressure. The eluent is dried over MgSO4, centrifuged, and aliquots are taken directly or diluted for GC/MS/MS and LC/MS/MS analysis, respectively. The entire process yields a 10× dilution factor relative to the original sample.

Použitá instrumentace

• Agilent 1290 Infinity II LC coupled to 6490 Triple Quadrupole LC/MS with Jet Stream ESI source
• Agilent 8890 GC with 7000E Triple Quadrupole GC/MS in dynamic MRM mode
• Agilent Bond Elut QuEChERS EN extraction kits
• Agilent Captiva EMR–LPD 6 mL cartridges
• Thermo centrifuge, SPE manifold, Geno/Grinder mixer

Main Results and Discussion

Captiva EMR–LPD cleanup removed approximately 60 % of co-extractives, yielding a cleaner chromatographic background than conventional dSPE. Using 1 g sample size, 95 % of targets achieved 70–120 % recoveries with average RSD<20 %, and >98 % of LC-amenable compounds exhibited matrix effects within 60–130 %. Matrix-matched calibration (10–5 000 ng/g) showed R²>0.99 for 88 % of pesticides. Cleanup comparisons demonstrated equivalent or improved performance versus two standard dSPE formulations, particularly for sensitive analytes.

Benefits and Practical Applications

The passthrough cleanup simplifies sample handling by eliminating tube transfers and centrifugation steps, reducing labor and turnaround time. It supports high-throughput monitoring of a broad pesticide panel in tobacco, facilitating compliance with regulatory standards and quality control in the food and beverage industry.

Future Trends and Applications

Emerging developments may integrate Captiva EMR–LPD cleanup with automated platforms for even greater throughput. Expansion to other challenging botanicals and the use of high-resolution mass spectrometry could further enhance selectivity. Data-driven approaches and AI-assisted processing are poised to streamline method development and real-time monitoring.

Conclusion

The combination of QuEChERS EN extraction and Captiva EMR–LPD passthrough cleanup delivers a robust, efficient workflow for simultaneous determination of over 300 pesticides in tobacco. The method meets stringent recovery, precision, and sensitivity criteria, offering a simplified alternative to traditional cleanups and supporting routine analytical demands.

References

• CORESTA GUIDE No. 1, Agrochemical Guidance Residue Levels, 2019.
• Leffingwell, J.C.; Basic Chemical Constituents of Tobacco Leaf and Differences among Tobacco Types; Blackwell Science, 1999.
• Rodgman, A.; Perfetti, T.A.; The Chemical Components of Tobacco and Tobacco Smoke; CRC Press, 2013.
• Bernardi, G.; et al.; An Effective Method for Pesticides Residues Determination in Tobacco by GC-MS/MS and UHPLC-MS/MS; Talanta 2016, 161, 40–47.
• Li, M.; et al.; Rapid Determination of Residual Pesticides in Tobacco by QuEChERS and LC-MS; J. Sep. Sci. 2013, 36, 2500–2529.
• Lee, J.-M.; et al.; Comparative Study of Pesticide Multi-residue Extraction in Tobacco for GC-MS/MS; J. Chrom. A 2008, 1187, 25–33.
• Andrianova, A.A.; Zhao, L.; Five Keys to 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.
• Zhao, L.; Wei, T.; Determination of Multiclass, Multiresidue Pesticides in Spring Leaf Mix Using Captiva EMR–HCF Cleanup and LC/MS/MS; Agilent Technologies Application Note 5994-4765EN.