Quantitative determination and validation of 17 cannabinoids in cannabis and hemp using liquid chromatography-tandem mass spectrometry

• Published in: Analytical and bioanalytical chemistry 2020-11, Vol.412 (27), p.7381-7393
• Main Authors: McRae, Garnet, Melanson, Jeremy E.
• Format: Article
• Language: English
• Subjects: ABC Highlights: authored by Rising Stars and Top Experts; Accuracy; Analysis; Analytical Chemistry; Biochemistry; Calibration; Cannabinoids; Cannabinoids - analysis; Cannabis; Cannabis - chemistry; Characterization and Evaluation of Materials; Chemistry; Chemistry and Materials Science; Chromatography; Chromatography, High Pressure Liquid - methods; Detection limits; Dilution; Dronabinol - analysis; Food Science; Hemp; Interrogation; Laboratory Medicine; Linearity; Liquid chromatography; Marijuana; Mass spectrometry; Mass spectroscopy; Medical marijuana; Methanol; Monitoring/Environmental Analysis; Paper in Forefront; Phenols; Plant Extracts - chemistry; Quality Control; Regression analysis; Scientific imaging; Spectroscopy; Tandem Mass Spectrometry - methods; Tetrahydrocannabinol
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-020-02862-8

The increase in production of cannabis for medical and recreational purposes in recent years has led to a corresponding increase in laboratories performing cannabinoid analysis of cannabis and hemp. We have developed and validated a quantitative liquid chromatography-tandem mass spectrometry (LC-MS/MS) method that is simple, reliable, specific, and accurate for the analysis of 17 cannabinoids in cannabis and hemp. Liquid-solid sample extraction coupled with dilution into a calibration range from 10 to 10,000 ng/mL and LC-MS/MS analysis provides quantification of samples ranging from 0.002 to 200 mg/g (0.0002 to 20.0%) in matrix. Linearity of calibration curves in methanol was demonstrated with regression r 2  ≥ 0.99. Within-batch precision (0.5 to 6.5%) and accuracy (91.4 to 108.0%) and between-batch precision (0.9 to 5.1%) and accuracy (91.5 to 107.5%) were demonstrated for quality control (QC) samples in methanol. Within-batch precision (0.2 to 3.6%) and accuracy (85.4 to 111.6%) and between-batch precision (1.4 to 6.1 %) and accuracy (90.2 to 110.3%) were also evaluated with a candidate cannabis certified reference material (CRM). Repeatability (1.5 to 12.4% RSD) and intermediate precision (2.2 to 12.8% RSD) were demonstrated via analysis of seven cannabis samples with HorRat values ranging from 0.3 to 3.1. The method provides enhanced detection limits coupled with a large quantitative range for 17 cannabinoids in plant material. It is suitable for a wide range of applications including routine analysis for delta-9-tetrahydrocannabinol (Δ 9 -THC), delta-9-tetrahydrocannabinolic acid (Δ 9 -THCA), cannabidiol (CBD), cannabidiolic acid (CBDA), and cannabinol (CBN) as well as more advanced interrogation of samples for both major and minor cannabinoids.