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Analysis of Twenty-Seven GC‑Amenable Pesticides Regulated in the Cannabis Industry in North America with the Agilent 8890/7010B Triple Quadrupole GC/MS System

Applications | 2020 | Agilent TechnologiesInstrumentation
GC/MSD, GC/MS/MS, GC/QQQ
Industries
Food & Agriculture
Manufacturer
Agilent Technologies

Summary

Importance of the Topic


Cannabis products require rigorous pesticide testing to comply with regulations and ensure consumer safety. Many GC-amenable pesticides present analytical challenges due to low required detection limits and complex plant matrices.

Study Objectives and Overview


This application note demonstrates a comprehensive workflow to detect and quantify 27 GC-amenable pesticides in dry cannabis flower, meeting or exceeding California Bureau of Cannabis Control and Health Canada requirements for limits of detection (LOD), limits of quantitation (LOQ), accuracy, and precision.

Methodology and Instrumentation


  • Instrument: Agilent 8890 GC coupled with 7010B Triple Quadrupole MS in electron ionization mode with High Efficiency Source, dynamic MRM, and retention time locking to the MassHunter Pesticide & Environmental Pollutant MRM database.
  • GC Configuration: Multimode inlet in cold solvent vent mode, dual 15 m HP-5MS UI columns in backflush setup, helium carrier gas, fast oven temperature program.
  • Sample Preparation: 1 g homogenized cannabis flower extracted with acetonitrile, cleaned via C18 SPE, final 125× dilution, two-layer sandwich injection.
  • Internal Standards: Parathion-d10 and α-BHC-d6 for analyte quantitation; triphenyl phosphate as surrogate standard for method performance monitoring.
  • Calibration and Quantitation: Matrix-matched calibration over 0.016–64 ppb in-vial, 5–8 levels per compound, 1/x weighting, statistical determination of MDL, LOD, and LOQ.

Main Results and Discussion


  • Empirical LOQs ranged from 0.009 to 1.488 ppb in-vial (0.69–186 ppb in-matrix), well below regulatory limits of 20–3000 ppb.
  • Calibration curves demonstrated excellent linearity (R² > 0.99) and accuracy within ±20% at reporting levels.
  • Recoveries for spiked quality controls were mostly between 70% and 130% across all analytes.
  • Precision remained robust over 114 sequential injections, with %RSD below 16% for representative pesticides.
  • Chromatographic backflush and dynamic MRM minimized matrix buildup and maintained stable performance.

Benefits and Practical Applications


  • Enables high-throughput, sensitive pesticide screening to meet stringent state and federal cannabis testing regulations.
  • Provides a unified sample preparation workflow for both GC/MS and LC/MS pesticide assays.
  • Supports quality assurance and product safety in medicinal and recreational cannabis laboratories.

Future Trends and Opportunities


  • Integration of high-resolution MS and automated sample preparation to enhance specificity and throughput.
  • Expansion to include additional non-GC-amenable pesticides and emerging contaminants using complementary LC/MS/MS methods.
  • Development of standardized inter-laboratory protocols and proficiency testing for cannabis analysis.

Conclusion


The optimized workflow using the Agilent 8890/7010B TQ GC/MS system achieves reliable detection and quantitation of 27 challenging pesticides in cannabis, exceeding California and Canadian regulatory requirements. The method offers robust performance, high sensitivity, and streamlined operations for routine pesticide testing.

References


  1. California Bureau of Cannabis Control. California Code of Regulations Title 16 Division 42. (2019).
  2. Health Canada. Mandatory Cannabis Testing for Pesticides Active Ingredients: List and Limits. (2019).
  3. Westland J., Andrianova A., Stone P. Optimizing Sample Preparation in Pesticides Analysis for Cannabis. Agilent Technologies Application Note 5994-0973EN. (2019).
  4. Hollis J.S., Andrianova A., Churley M. Analysis of Challenging Pesticides in Cannabis and Hemp with the Agilent Intuvo 9000/7010 GC/MS/MS: Fast-5. Agilent Technologies Application Note 5994-1604EN. (2019).
  5. Honnold R. et al. A Fast Analysis of the GC/MS/MS Amenable Pesticides Regulated by the California Bureau of Cannabis Control. Agilent Technologies Application Note 5994-1019. (2019).
  6. Andrianova A., Westland J. Sensitive Detection of Pesticides Regulated in California in Dried Cannabis Plant Material. Agilent Technologies Application Note 5994-0568EN. (2019).
  7. Stone P.J.W. et al. Determination of Pesticides and Mycotoxins in Cannabis Flower by Triple Quadrupole LC/MS/MS. Agilent Technologies Application Note 5994-1743EN. (2020).
  8. Stone P.J.W. et al. Determination of Pesticides and Mycotoxins in Cannabis Flower Defined by California Recreational Cannabis Regulations. Agilent Technologies Application Note 5994-0648EN. (2019).
  9. Roy J-F. et al. A Sensitive and Robust Workflow to Measure Residual Pesticides and Mycotoxins from the Canadian Target List in Dry Cannabis Flower. Agilent Technologies Application Note 5994-0429EN. (2018).
  10. Macherone A. Tackle Emerging Cannabis Regulations with Confidence: Why LC/MS/MS and GC/MS/MS Are Required for the Analysis of Certain Pesticides. Agilent Technologies Application Note 5994-1127EN. (2019).
  11. Mastovska K. Rugged GC/MS/MS Pesticide Residue Analysis Fulfilling the USDA Pesticide Data Program Requirements. Agilent Technologies Application Note 5991-1054EN. (2012).
  12. Agilent Technologies. GC/MS/MS Pesticide Residue Analysis Reference Guide. 5991-2389EN. (2018).

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