Simultaneous determination of LSD and 2-oxo-3-hydroxy LSD in hair and urine by LC–MS/MS and its application to forensic cases

• Published in: Journal of pharmaceutical and biomedical analysis 2015-11, Vol.115, p.138-143
• Main Authors: Jang, Moonhee, Kim, Jihyun, Han, Inhoi, Yang, Wonkyung
• Format: Article
• Language: English
• Subjects: 2-oxo-3-hydroxy-LSD; Adolescent; Chromatography, Liquid - instrumentation; Chromatography, Liquid - methods; Forensic Toxicology - instrumentation; Forensic Toxicology - methods; Hair; Hair - chemistry; Humans; Limit of Detection; Liquid chromatography–tandem mass spectrometry; LSD; Lysergic Acid Diethylamide - analogs & derivatives; Lysergic Acid Diethylamide - analysis; Lysergic Acid Diethylamide - urine; Male; Middle Aged; Reproducibility of Results; Spectrometry, Mass, Electrospray Ionization - instrumentation; Spectrometry, Mass, Electrospray Ionization - methods; Tandem Mass Spectrometry - instrumentation; Tandem Mass Spectrometry - methods; Urine
• ISSN: 0731-7085; 1873-264X
• DOI: 10.1016/j.jpba.2015.07.001

[Display omitted] •LC–MS/MS methods were developed to document LSD use in hair and urine specimens.•Target analytes were LSD and its metabolite, 2-oxo-3-hydroxy-LSD.•The methods showed good sensitivity for both analytes with a small amount of sample.•The methods were successfully applied to authentic specimens from LSD intake cases. Lysergic acid diethylamide (LSD) is administered in low dosages, which makes its detection in biological matrices a major challenge in forensic toxicology. In this study, two sensitive and reliable methods based on liquid chromatography–tandem mass spectrometry (LC–MS/MS) were established and validated for the simultaneous determination of LSD and its metabolite, 2-oxo-3-hydroxy-LSD (O-H-LSD), in hair and urine. Target analytes in hair were extracted using methanol at 38°C for 15h and analyzed by LC–MS/MS. For urine sample preparation, liquid–liquid extraction was performed. Limits of detection (LODs) in hair were 0.25pg/mg for LSD and 0.5pg/mg for O-H-LSD. In urine, LODs were 0.01 and 0.025ng/ml for LSD and O-H-LSD, respectively. Method validation results showed good linearity and acceptable precision and accuracy. The developed methods were applied to authentic specimens from two legal cases of LSD ingestion, and allowed identification and quantification of LSD and O-H-LSD in the specimens. In the two cases, LSD concentrations in hair were 1.27 and 0.95pg/mg; O-H-LSD was detected in one case, but its concentration was below the limit of quantification. In urine samples collected from the two suspects 8 and 3h after ingestion, LSD concentrations were 0.48 and 2.70ng/ml, respectively, while O-H-LSD concentrations were 4.19 and 25.2ng/ml, respectively. These methods can be used for documenting LSD intake in clinical and forensic settings.