A fast and reliable UPLC-MS/MS method was developed and validated for measuring dimethyltryptamine (DMT) in hair samples. The method, which pulverizes 20-milligram hair samples with methanol below 4 °C, achieved a lower limit of quantitation of 3 pg/mg and a calibration curve with R² = 0.992. Intraday and interday precision (RSD < 15%) and accuracy (92-113%) were acceptable, and dilution integrity was confirmed. Applied to 28 forensic cases, DMT concentrations ranged from 3 to 1109 pg/mg.
A highly sensitive method for measuring psilocin and psilocybin in hair samples from magic mushroom users was developed using ultra-high pressure liquid chromatography coupled with tandem mass spectrometry. The technique achieved a detection limit of 1 pg/mg and a quantification limit of 5 pg/mg, with linear calibration from 5 to 500 pg/mg. In two authentic hair samples, psilocin concentrations were 161 and 150 pg/mg, while psilocybin was not detected. The method also analyzed psilocin and psilocybin distribution in seven hallucinogenic mushrooms. This represents the first measurement of psilocin in hair from hallucinogenic mushroom consumers and the most sensitive quantitative method for these compounds in hair.