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Analysis of Challenging Pesticides Regulated in the Cannabis and Hemp Industry with the Agilent Intuvo 9000‑7010 GC/MS/MS system: The Fast-5

Applications | 2019 | Agilent TechnologiesInstrumentation
GC/MSD, GC/MS/MS, GC/QQQ
Industries
Food & Agriculture
Manufacturer
Agilent Technologies

Summary

Importance of the Topic


Residual pesticide testing in cannabis and hemp is essential to ensure consumer safety and legal compliance. Regulatory bodies in the US and Canada list nearly 100 pesticides, of which pentachloronitrobenzene (PCNB), methyl parathion, captan, chlordane isomers, and chlorfenapyr (the Fast-5) pose particular analytical challenges due to low detection limits and complex sample matrices such as flowers, concentrates, and edibles.

Aims and Study Overview


This study presents a streamlined GC/MS/MS method using the Agilent Intuvo 9000-7010B system to identify and quantify the Fast-5 pesticides in diverse cannabis matrices. The primary objectives are to achieve detection limits and quantification limits that satisfy stringent regulatory requirements, while demonstrating accuracy, precision, linearity, and robustness in a single analytical workflow.

Methodology


  • Sample Preparation: Modified QuEChERS extraction from 1 g homogenized cannabis flower, followed by C18 SPE cleanup and dilution steps to yield a final 125-fold sample dilution.
  • Analyte Protectants: A two-layer sandwich injection of analyte protectants (L-gulonolactone and D-sorbitol) to minimize matrix effects and improve peak shape.
  • Calibration and Quality Control: Eight-level matrix-matched calibration (0.016–64 ppb) with isotopically labeled internal standards (α-BHC-d6, parathion-d10) and triphenyl phosphate as a surrogate.
  • Statistical Evaluation: Use of MassHunter Quant-My-Way package to calculate LOD, LOQ, accuracy, precision, and linearity based on replicate injections (n=5) and three independent datasets.

Použitá instrumentace


  • Gas Chromatograph: Agilent Intuvo 9000 with 7693 autosampler, MultiMode Inlet (MMI), mid-column backflush flow chip, Guard Chip, and two Agilent J&W HP-5MS UI columns (15 m × 0.25 mm, 0.25 µm).
  • Tandem Mass Spectrometer: Agilent 7010B with High Efficiency Source (HES) in EI mode, operated with explicit MRM time segments.
  • Software: Agilent MassHunter Workstation B.10 with Acquisition, Qualitative, Quantitative, and Quant-My-Way Cannabis UI packages.

Results and Discussion


The Fast-5 method demonstrated:
  • Empirical LODs: 0.019–0.26 ppb in matrix, well below regulatory limits.
  • Empirical LOQs: 0.51–4.37 ppb in matrix, complying with California and Health Canada thresholds.
  • Linearity: R2 > 0.998 across the tested range for all analytes.
  • Accuracy: Intraday and interday quantitation accuracy between 86–113% for individual compounds and total chlordane.
  • Precision: Relative standard deviation (RSD) ≤10% for all analytes over multiple days.

Benefits and Practical Applications


  • Single-method solution covering multiple challenging pesticides in various cannabis and hemp products.
  • High selectivity and sensitivity reduces false positives and ensures reliable compliance reporting.
  • Eco-friendly design with minimal solvent use and simplified consumables management.
  • Scalable workflow supports routine high-throughput testing in quality control laboratories.

Future Trends and Possibilities


As cannabis regulations evolve, the method can be extended to additional pesticide classes and emerging contaminants. Integration with automated sample preparation, high-resolution MS, and data analytics will further enhance throughput and data quality, enabling faster decision-making in research, industrial quality assurance, and regulatory enforcement.

Conclusion


The Agilent Intuvo 9000-7010B GC/MS/MS Fast-5 method delivers robust, accurate, and precise analysis of five challenging pesticides in cannabis and hemp matrices. Its validated performance metrics and streamlined workflow meet current regulatory requirements and support reliable routine testing.

Reference


  • Curtis M. et al. Cannabis Science and Technology 2019, 2(5):56–60, 70.
  • Honnold R.; Fausett E.; Westland J.; Macherone A. Agilent Technologies Application Note 5994-1019, 2019.
  • AOAC Official Method 2007.01. Pesticide Residues in Foods by Acetonitrile Extraction and Partitioning with Magnesium Sulfate. AOAC International, 2007.
  • Bureau of Cannabis Control. California Code of Regulations Title 16 Division 42. Retrieved October 2019.
  • Stone P.J.W. et al. Agilent Technologies Application Note 5994-0648EN, 2019.

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