Rapid quantification of cannabinoids in beef tissues and bodily fluids using direct-delivery electrospray ionization mass spectrometry

Authors: CHAKRABARTY, SHUBHASHIS - North Dakota State University; Serum, Eric; WINDERS, THOMAS - North Dakota State University; Neville, Bryan; KLEINHENZ, MICHAEL - Kansas State University; MAGNIN, GERALDINE - Kansas State University; COETZEE, JOHANN - Kansas State University; DAHLEN, CARL - North Dakota State University; SWANSON, KENDALL - North Dakota State University; Smith, David

Submitted to: Food Additives & Contaminants
Publication Type: Peer Reviewed Journal
Publication Acceptance Date: 7/21/2022
Publication Date: 8/8/2022
Citation: Chakrabarty, S., Serum, E.M., Winders, T.M., Neville, B.W., Kleinhenz, M.D., Magnin, G., Coetzee, J.F., Dahlen, C.R., Swanson, K.C., Smith, D.J. 2022. Rapid quantification of cannabinoids in beef tissues and bodily fluids using direct-delivery electrospray ionization mass spectrometry. Food Additives & Contaminants. https://doi.org/10.1080/19440049.2022.2107711.
DOI: https://doi.org/10.1080/19440049.2022.2107711

Interpretive Summary: Hempseed cake is a byproduct of hempseed oil extraction and is potentially a useful source of protein and fiber in cattle, sheep, and poultry diets. Because levels of biologically active residues (cannabinoids) have not been measured in meat products after feeding hemp or its byproducts, hemp ingredients are not allowed in diets of food animals. A major limitation to investigating such residues is the lack of a rapid and sensitive analytical method capable of quantifying cannabinoids in meats. To this end, a mass-spectrometric method for simultaneously quantifying 10 cannabinoid residues in cattle tissues, plasma, and urine was developed and validated. The method was sensitive with limits of detection generally being less than 3 parts per billion; the method was also rapid, requiring mass spectrometric instrument time of only 1 minute per sample. The rapid method returned no false positives for cannabinoids in plasma, urine, liver, or skeletal muscle samples from 6 control cattle (90 samples). Results of the analysis of cannabinoids in plasma of cattle fed hemp flowers were highly correlated with results derived from traditional analytical methods. The rapid method has great potential for use in quantifying cannabinoid residues in livestock fed industrial hemp or industrial hemp byproducts.

Technical Abstract: Hempseed cake is a byproduct of hempseed oil extraction and is potentially a useful source of protein and fiber for use in ruminant diets. However, data are lacking on the appearance and/or clearance of cannabinoids in tissues of animals fed hempseed cake. To this end, a rapid method for quantifying cannabinol (CBN), cannabidiol (CBD), cannabinolic acid (CBNA), cannabidiolic acid (CBDA), cannabigerolic acid (CBGA), cannabichromenic acid (CBCA), cannabidivarin (CBDV), cannabidivarinic acid (CBDVA), tetrahydrocannabinol (THC) and tetrahydrocannabinolic acid (THCA) in cattle tissues, plasma, and urine was developed using rapid screen electrospray ionization mass spectrometry (RS-ESI-MS). Regression coefficients of matrix-matched standard curves ranged from 0.9946 to >0.9999 and analyte recoveries averaged from 90.2 ± 15.5 to 108.7 ± 18.7% across all compounds. Limits of detection and quantification ranged from 0.05 to 2.79 ng/mL and 0.17 to 9.30 ng/mL, respectively, while the inter-day relative standard deviation ranged from 5.1 to 15.1%. Rapid screening electrospray ionization mass spectrometry (RS-ESI-MS) returned no false positives for any cannabinoid in plasma, urine, and tissue (liver, skeletal muscle) samples from 6 non-dosed control animals (n = 90 samples; of which 72 samples were plasma or urine and 18 samples were tissues). Across-animal cannabinoid concentrations measured in 32 plasma samples of cattle dosed with ground hemp were quantified by RS-ESI-MS; analytical results correlated well (r2 = 0.963) with independent LC-MS/MS analysis of the same samples.