Analysis of Psilocin, Bufotenine and LSD in Hair

Abstract

A method for the simultaneous extraction of the hallucinogens psilocin, bufotenine, lysergic acid diethylamide (LSD) as well as iso-LSD, nor-LSD and O-H-LSD from hair with hydrochloride acid and methanol is presented. Clean-up of the hair extracts is performed with solid phase extraction using a mixed-mode cation exchanger. Extracts are measured with liquid chromatography coupled with electrospray tandem mass spectrometry. The method was successfully validated according to the guidelines of the 'Society of Toxicological and Forensic Chemistry' (GTFCh). To obtain reference material hair was soaked in a solution of the analytes in dimethyl sulfoxide/methanol to allow incorporation into the hair. These fortified hair samples were used for method development and can be employed as quality controls.

Toxicology and Analysis of Psychoactive Tryptamines

“…Table 2 summarizes the analytical methods reported for the determination of tryptamines in biological matrices, including information on sample size, sample preparation, instrumentation and validation parameters. Different biological matrices were employed for forensic purposes including conventional matrices urine [102,112,114,118,[121][122][123]125,126], blood [110,[113][114][115][117][118][119]121,123], plasma [109,111,112,118] serum [112] and unconventional matrices oral fluid [120] and hair [116,124]. Protein precipitation is a simple sample preparation method, providing sufficient extraction efficiency while simplifying extraction and preparation time.…”

“…Different protein precipitation methods [115,117,119,121] include different solvents for blood extraction but methanol is the most common solvent. Different sample preparation techniques include protein precipitation [113,116,117,119] for urine, serum and blood samples, acid hydrolysis [102,121,122] for urine, centrifugation [102,111,112,[114][115][116][117]119,[121][122][123][124]126] for blood, plasma and urine samples, washing [109,114,116,125] for plasma, blood and hair samples, enzymatic hydrolysis for urine samples [112], solid phase extraction (SPE) [109][110][111]114], liquid-liquid extraction (LLE) [114,120], dispersive liquid-liquid microextraction (DLLME) [115] and a solvent extraction for dried blood spots (DBS) [113]. Tryptamine is a relatively labile analyte but it remains stable in an acidic environment.…”

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

“…To our knowledge, there are only two reports on LSD detection in head hair samples [17,18]. However, in those reports, the samples were analyzed using GC-MS or HPLC with a fluorescence detector.…”

“…With improvements in instrumental techniques, analytical methods employing mass spectrometry have been developed for the detection of LSD or/and its metabolites at low concentrations in various biological matrices [10][11][12][13][14][15][16][17]. However, studies on the analysis of LSD and its metabolites in hair are limited in comparison with those in urine or blood.…”

“…In addition, Gaulier et al [20] detected LSD in pubic hair from an LSD-related postmortem case using liquid chromatography-tandem mass spectrometry (LC-MS/MS). More recently, an LC-MS/MS method was developed and validated for the analysis of hallucinogens including LSD, iso-LSD, nor-LSD, and O-H-LSD in hair [17]. However, the method's application to authentic samples for demonstrating its feasibility was not carried out.…”