Determination of Over 300 Pesticides in Tobacco

Importance of the Topic

Tobacco is a complex and globally consumed product that may carry pesticide residues from cultivation and storage. Reliable methods for multiresidue analysis are essential to ensure compliance with regulatory limits and protect public health.

Study Objectives and Overview

This work presents a streamlined workflow to detect over 300 pesticides in tobacco. It integrates QuEChERS extraction with Agilent Captiva EMR–LPD passthrough cleanup, followed by analysis on LC/MS/MS and GC/MS/MS platforms. The goal is to achieve efficient matrix removal, accurate quantitation, and low failure rates.

Methodology

• Sample Preparation: 1 g of ground tobacco is hydrated with aqueous buffer and extracted with acetonitrile containing 1 % acetic acid and QuEChERS salt packet.
• Cleanup: A 3 mL aliquot of crude extract is processed through a 6 mL Captiva EMR–LPD cartridge under gentle pressure for pigment and lipid removal.
• Eluate Treatment: The cleaned extract is dried with anhydrous MgSO₄ and directly used for GC/MS/MS or diluted fivefold for LC/MS/MS.

Used Instrumentation

• LC/MS/MS: Agilent 1290 Infinity II LC coupled to 6490 triple quadrupole with Jet Stream electrospray source.
• GC/MS/MS: Agilent 8890 GC with 7000E triple quadrupole, multimode inlet, and midcolumn backflush.
• Software: Agilent MassHunter Workstation using dynamic MRM acquisition.

Main Results and Discussion

• Matrix Removal: Approximately 60 % of co-extractives removed, confirmed by residual weight and cleaner chromatographic background.
• Quantitation Performance: Over 95 % of pesticides showed recoveries between 70 % and 120 %, with <20 % RSD for >98 % of targets at 20 and 100 ng/g spiking levels.
• Calibration Linearity: For 84 % of compounds, a linear range of 10–5 000 ng/g in tobacco achieved R² > 0.99; about 4 % required quadratic fitting.
• Cleanup Comparison: Captiva EMR–LPD matched or outperformed two common dSPE approaches in recovery, reproducibility, and matrix effects while reducing handling steps.

Benefits and Practical Applications

• Comprehensive Coverage: Simultaneous analysis of >300 LC- and GC-amenable pesticides.
• Efficiency: Passthrough cleanup simplifies workflow and reduces labor compared to dispersive SPE.
• High Data Quality: Consistent recoveries, low RSDs, and minimal matrix effects support regulatory and quality-control testing.
• Versatility: Suitable for routine pesticide monitoring in tobacco and other complex botanical matrices.

Future Trends and Potential Applications

Expanding this approach to other dry botanical matrices using targeted EMR cartridges can enhance applicability. Integration with automated sample preparation and high-resolution mass spectrometry may further boost throughput and extend analyte scope. Ongoing sorbent development will improve cleanup efficiency for challenging compounds.

Conclusion

The combined QuEChERS extraction and Captiva EMR–LPD passthrough cleanup deliver a rapid, reliable method for multiresidue pesticide analysis in tobacco. Demonstrated matrix removal and excellent quantitation performance enable confident screening of over 300 compounds by LC/MS/MS and GC/MS/MS.

References

• CORESTA GUIDE No. 1, Agrochemical Guidance Residue Levels, 2019.
• Leffingwell JC et al., Basic Chemical Constituents of Tobacco Leaf, Tobacco: Production, Chemistry and Technologies, 1999.
• Rodgman A; Perfetti TA, The Chemical Components of Tobacco, CRC Press, 2013.
• Bernardi G et al., Talanta 2016, 161, 40–47.
• Li M et al., J. Sep. Sci. 2013, 36, 2500–2529.
• Lee J-M et al., J. Chrom. A 2008, 1187, 25–33.