Hemp seeds and hempseed oil are marketed on- and off-line as health foods and cosmetics and have beenreported to have high nutrient contents. However, because of the various side effects of cannabinoids,especially49-tetrahydrocannabinol (THC), many countries regulate upper limits for THC in products,which creates the need for analytical techniques capable of measuring THC, cannabidiol (CBD), andcannabinol (CBN) levels in commercial hemp seeds and hempseed oil. In the present study, hemp seedand hempseed oil extracts obtained by methanol extraction, were analyzed by gas chromatography–mass spectrometry (GC/MS). Validation of the technique used was performed using calibration curvesand by determining LODs, LOQs, specificities, selectivities, and intra- and inter-day precision andaccuracies. In addition, matrix effects, process efficiencies, recoveries, and sample stabilities wereinvestigated. In hemp seeds, as determined using the fully optimized method THC concentrations rangedfrom 0.06 to 5.91 mg/g, CBD concentrations from 0.32 to 25.55 mg/g, and CBN concentrations from 0.01 to1.50 mg/g; CBN/THC ratios ranged from 0.1 to 1.60, and CBD/THC ratios from 0.11 to 62.56. Furthermore,the (THC + CBN)/CBD ratio of most hemp seed samples was less than one. In hempseed oil, THCconcentrations ranged from 0.3 to 19.73 mg/mL, CBD concentrations from 6.66 to 63.40 mg/mL, CBNconcentrations from 0.11 to 2.31 mg/mL, CBN/THC ratios from 0.12 to 0.42, and CBD/THC ratios from 3.21to 22.50. Furthermore, (THC + CBN)/CBD ratios in all hempseed oil samples were less than one. Theoptimized methanol extraction-GC/MS technique was found to be satisfactory for determining THC, CBD,and CBN concentrations in hemp seeds and hempseed oil.
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