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A simple and sensitive assay for the cannabinoids is presented using a dabsylation procedure. Dabsyl derivatives of Δ9-tetrahydrocannabinol (Δ9-THC) and cannabinol (CBN) were prepared by reacting with 4-dimethylaminoazobenzene-4'-sulfonyl chloride (dabsyl chloride) in acetone in the presence of sodium carbonate-sodium bicarbonate buffer (pH 10). Crystalline dabsylcannabinoids gave intense absorption in the visible region. With these derivatives, analysis by thin-layer chromatography (TLC) and high performance liquid chromatography (HPLC) were tested. These techniques gave good separation and nanogram detection of dabsyl-THC and -CBN by using n-hexane-ethyl acetate-diethylamine (20: 5: 1) for TLC and MeOH—H20 (95 : 5) at 450 nm for HPLC.