Meeting California Cannabis Regulations with the Agilent 1260 Infinity II Prime LC and Agilent Ultivo Triple Quadruple MS

Význam tématu

The legalization of cannabis in multiple jurisdictions has driven a critical need for reliable, streamlined testing methods to ensure product safety and regulatory compliance. California regulations mandate the determination of over 50 LC/MS-amenable pesticides, key mycotoxins, and major cannabinoids for potency, traditionally requiring separate workflows. Integrating these analyses into a single method accelerates turnaround, reduces resource burden, and supports quality control in licensed testing laboratories.

Cíle a přehled studie / článku

This Application Note presents a unified workflow using the Agilent 1260 Infinity II Prime LC coupled to the Ultivo Triple Quadrupole MS for simultaneous quantitation of regulated pesticides, four aflatoxins, ochratoxin A, and six principal cannabinoids in cannabis flower. The goal is to validate detection limits, accuracy, precision, and robustness, demonstrating compliance with California action levels in one extraction and one LC/MS run.

Použitá metodika a instrumentace

Sample preparation begins with grinding 1 g of cannabis flower, extraction in acetonitrile, simple SPE cleanup, and a 250× dilution. Calibration employs 12C standards for pesticides and mycotoxins, and 13C isotopic transitions for cannabinoids to prevent detector saturation. Chromatographic separation is achieved on an Agilent Poroshell 120 EC-C18 column over an 8-minute gradient, with injections of 2 µL. MS/MS analysis uses dynamic MRM with alternating positive/negative polarity allowing concurrent monitoring of all analytes.

Instrumentace

• Agilent 1260 Infinity II Prime LC (flexible pump, multisampler, multicolumn thermostat)
• Agilent Ultivo Triple Quadrupole LC/MS with dynamic MRM and fast polarity switching
• SPE cartridges (200 mg/6 mL polymeric reversed-phase), HPLC-grade solvents, and certified reference standards

Hlavní výsledky a diskuse

The workflow meets California LOQs (100 ppb for pesticides, 20 ppb for mycotoxins, percent levels for cannabinoids). Recoveries in matrix: 75–105% for pesticides, 60–80% for mycotoxins, and 85–105% for cannabinoids via isotopic calibration. Chromatographic peaks are 3–5 s wide, ensuring clear resolution. Robustness testing over 80 sequential injections demonstrated consistent performance. Analysis of real cannabis samples detected imidacloprid below the 5 ppm limit and confirmed absence of regulated mycotoxins.

Přínosy a praktické využití metody

• Consolidates potency, pesticide, and mycotoxin testing into one protocol, reducing hands-on time and solvent consumption
• Employs MS/MS specificity and 13C calibration for high-abundance cannabinoids without sacrificing sensitivity for trace contaminants
• Supports regulatory compliance and efficient resource utilization in cannabis testing laboratories

Budoucí trendy a možnosti využití

Expansion of the analyte panel to include GC/MS-amenable pesticides, automation of sample preparation, and application to other botanical matrices are promising next steps. Continued development of multiplexed LC/MS workflows will enhance throughput and further streamline quality assurance in the cannabis and hemp industries.

Závěr

The described single-method workflow effectively quantifies regulated pesticides, key mycotoxins, and cannabinoids in cannabis flower, meeting stringent California requirements with high accuracy, precision, and throughput. This integrated LC/MS/MS approach represents a powerful platform for laboratories seeking to optimize analytical efficiency and compliance.

Reference

1. FDA approves first drug comprised of an active ingredient derived from marijuana to treat rare, severe forms of epilepsy. FDA, 2018.
2. California Proposition 215 (Compassionate Use Act).
3. California Proposition 64 (Adult Use of Marijuana Act), 2016.
4. California Department of Pesticide Regulation. Pesticides Legal to Use on Cannabis, 2018.
5. California Department of Pesticide Regulation. Cannabis Pesticides That Cannot Be Used.
6. California Bureau of Cannabis Control. Title 16, Regulations Text, 2018.
7. Asanuma L. et al. Agilent Application Note 5991-9030EN, 2018.
8. Roy J.-F. et al. Agilent Application Note 5994-0429EN, 2018.
9. Stone P. J. et al. Agilent Application Note 5994-0648EN, 2019.
10. Christy S., Zumwalt M., Macherone A. Agilent Application Note 5991-9285EN, 2018.