An innovative approach for selective and robust screening of NBOHs, NBOMes, and LSD in forensic samples using a 3D-Printed electrochemical double cell.

Lysergic acid diethylamide (LSD) and two phenethylamine classes (NBOHs and NBOMes) are the main illicit drugs found in seized blotter papers. The preliminary identification of these substances is of great interest for forensic analysis. In this context, this work constitutes the inaugural demonstration of an efficient methodology for the selective detection of LSD, NBOHs, and NBOMes, utilizing a fully 3D-printed electrochemical double cell (3D-EDC). This novel 3D-EDC enables the use of two working electrodes and/or two supporting electrolytes (at different pHs) in the same detection system, with the possibility of shared or individual auxiliary and pseudo-reference electrodes. Thus, the selective voltammetric detection of these substances is proposed using two elegant strategies: (i) utilizing the same 3D-EDC platform with two working electrodes (boron-doped diamond (BDD) and 3D-printed graphite), and (ii) employing two pH levels (4.0 and 12.0) with 3D-printed graphite electrode. This comprehensive framework facilitates a fast, robust, and uncomplicated electrochemical analysis. Moreover, this configuration enables a rapid and sensitive detection of LSD, NBOHs, and NBOMes in seized samples, and can also provide quantitative analysis. The proposed method showed good stability of the electrochemical response with RSD <9 % for Ip and <5 % for Ep, evaluating all oxidation processes observed for studied analytes (n = 7) at two pH levels, using the same and different (n = 3) working electrodes. It demonstrates a broad linear range (20-100 and 20-70 µmol L-1) and a low LOD (1.0 µmol L-1) for quantification of a model molecule (LSD) at the two pHs studied. Hence, the 3D-EDC combined with voltammetric techniques using BDD and 3D-printed graphite electrodes on the same platform, or only with this last sensor at two pH values, provide a practical and robust avenue for preliminary identification of NBOHs, NBOMes, and LSD. This method embodies ease, swiftness, cost-efficiency, robustness, and selectivity as an on-site screening tool for forensic analysis.

A simple, quick and non-destructive approach for sampling drugs of abuse in tablets and blotter for qualitative analysis by paper spray mass spectrometry.

This study presents the development of a simple, fast, and inexpensive approach for the direct analysis of new psychoactive substances (NPS) in seized tablets and blotter paper, with improved sample preservation and increased analytical frequency. Paper triangles were gently rubbed against the surface of the samples containing synthetic drugs and then subjected to analysis by paper spray ionization mass spectrometry (PS-MS). Seized samples containing lysergic acid diethylamide (LSD) and several other substances from the classes of amphetamines, N-benzyl-substituted phenethylamines, synthetic cathinones, and synthetic cannabinoids, were analysed. Three types of paper were tested (filter paper, blotter paper, and synthetic paper) and several combinations of spray solvents were studied for the optimization. All samples were weighed and photographed before and after sequences of analysis in order to attest to the sample preservation. The results revealed that the approach is excellent for sample preservation, with less than 5% of mass loss even after 27 consecutive analyses. Moreover, no significant signal decreases were observed in mass spectrometry (MS) even after the experiments. It was possible to unequivocally identify illicit substances from seized samples (pills and blotter paper). By overcoming the solubilization and wet extraction process used for sample preparation, the waste was restricted to a volume of only 10 µL of solvent for the PS-MS analysis. The main advantage of our approach over existing methods is the sample preparation, which is simple and quick since the samples are just rubbed against the PS paper. This brings enormous benefits in terms of analytical frequency, economy of time and low consumption of solvents. Another important point is that the sample can remain intact for further analysis, which is crucial in forensic analysis.

Comprehensive detection of lysergic acid diethylamide (LSD) in forensic samples using carbon nanotube screen-printed electrodes.

Lysergic acid diethylamide (LSD) is a prevalent psychoactive substance recognized for its hallucinogenic properties, often encountered in blotter papers for illicit consumption. Given that LSD ranks among the most widely abused illicit drugs globally, its prompt identification in seized samples is vital for forensic investigations. This study presents, for the first time, an electrochemical screening method for detecting LSD in forensic samples, utilizing a multi-wall carbon nanotube screen-printed electrode (SPE-MWCNT). The LSD detection process was optimized on SPE-MWCNT in a phosphate buffer solution (0.1 mol L-1, pH 12.0) using square wave voltammetry (SWV). The combined use of SPE-MWCNT with SWV displayed robust stability in electrochemical responses for both qualitative (peak potential) and quantitative (peak current) LSD assessment, with a relative standard deviation (RSD) of less than 5% across the same or different electrodes (N = 3). A linear detection range was established between 0.16 and 40.0 µmol L-1 (R2 = 0.998), featuring a low limit of detection (LOD) of 0.05 µmol L-1. Interference studies with twenty-three other substances, including groups of phenethylamines typically found in blotting papers (e.g., NBOHs and NBOMes) and traditional illicit drugs, were performed, revealing a highly selective response for LSD using the proposed method. Consequently, the integration of SPE-MWCNT with SWV offers a robust tool for qualitative and quantitative LSD analysis in forensic applications, providing rapid, sensitive, selective, reproducible, and straightforward preliminary identification in seized samples.

Stability studies of ALD-52 and its homologue 1P-LSD.

With the emergence of new psychoactive substances (NPSs) over the years, the substances detected on stamps (also known as blotter papers) have also evolved from the traditional drug-lysergic acid diethylamide (LSD) to the multiple variants of lysergamides such as ALD-52 and 1P-LSD. The analysis of such blotter papers is usually done by solvent extraction followed by identification using gas chromatography-mass spectrometry (GC-MS). This study has shown that hydrolysis to form LSD was observed in GC-MS analysis when ALD-52 was extracted with methanol. The extraction of ALD-52 using other solvents such as acetonitrile, ethanol, isopropyl alcohol, ethyl acetate, and acetone, followed by GC-MS analysis, was investigated. It is shown that alcoholic solvents such as methanol and ethanol will result in the conversion of ALD-52 to LSD during GC-MS analysis, whereas the sterically hindered isopropyl alcohol will prevent this conversion. Investigation also shows that the hydrolysis of ALD-52 to LSD occurs at the GC injector port. It was also observed that the degree of hydrolysis was more pronounced at a lower concentration (0.1 mg/mL). The study was extended to a close analog-1P-LSD, and the results showed that 1P-LSD similarly hydrolyzes to LSD. However, 1P-LSD was observed to be more stable than ALD-52 due to steric hindrance because of the propanoyl group.

Quantitative Analysis of Lysergic Acid Diethylamide and Metabolite in Urine by Automated Extraction and Liquid Chromatography-Tandem Mass Spectrometry.

Recently, lysergic acid diethylamide (LSD) has become a resurgent drug of abuse. The detection of LSD is problematic because of the low dosage taken by users, light and heat sensitivity of the analyte and the lack of efficient analytical methods. Presented here is the validation of an automated sample preparation method for the analysis of LSD and its primary urinary metabolite, 2-oxo-3-hydroxy-LSD (OHLSD), in urine samples by liquid chromatography-tandem mass spectrometry. Analytes were extracted from urine using an automated Dispersive Pipette XTRaction method on Hamilton STAR and STARlet liquid handling systems. The limit of detection for both analytes was administratively defined at the lowest calibrator used in the experiments, and the limit of quantitation was 0.05 ng/mL for both analytes. All validation criteria were acceptable per Department of Defense Instruction 1010.16 requirements. This method offers an efficient, sensitive analytical solution to routinely evaluate large numbers of urine specimens for LSD in workplace drug deterrence programs.

[Identification of LSD Derivatives, 1cP-LSD, MIPLA and 1B-LSD in Illegal Products as Paper Sheet].

Lysergic acid diethylamide (LSD) is a hallucinogen, synthesized from ergot alkaloid, and controlled as a narcotic in Japan. Recently, LSD derivatives have appeared as designer drugs, all over the world. In previous study, we reported identification and analysis of four LSD derivatives in four paper sheet products. In this study, we detected three additional LSD derivatives from three paper sheet products, which were obtained from September 2019 to March 2020 in Japan. We extracted the compounds from paper sheet products with methanol for LC-MS, high-resolution MS and GC-MS analyses. The compounds were identified as 4-cyclopropionyl-N,N-diethyl-7-methyl-4,6,6a,7,8,9-hexahydroindolo[4,3-fg]quinoline-9-carboxamide (1cP-LSD), N-methyl-N-isopropyl-7-methyl-4,6,6a,7,8,9-hexahydroindolo-[4,3-fg]quinoline-9-carboxamide (MIPLA), 4-butyryl-N,N-diethyl-7-methyl-4,6,6a,7,8,9-hexahydroindolo[4,3-fg]quinoline-9-carboxamide (1B-LSD), by GC-MS, LC-MS, LC-Q-TOF-MS and NMR analyses. As well as other N1-acylated LSD derivatives, 1cP-LSD and 1B-LSD were easily deacylated to LSD during GC-MS analysis, we have to be careful to analyze these compounds.

Development of a Pencil Drawn Paper-based Analytical Device to Detect Lysergic Acid Diethylamide (LSD)*, †.

The need for agile and proper identification of drugs of abuse has encouraged the scientific community to improve and to develop new methodologies. The drug lysergic acid diethylamide (LSD) is still widely used due to its hallucinogenic effects. The use of voltammetric methods to analyze narcotics has increased in recent years, and the possibility of miniaturizing the electrochemical equipment allows these methods to be applied outside the laboratory; for example, in crime scenes. In addition to portability, the search for affordable and sustainable materials for use in electroanalytical research has grown in recent decades. In this context, employing paper substrate, graphite pencil, and silver paint to construct paper-based electrodes is a great alternative. Here, a paper-based device comprising three electrodes was drawn on 300 g/m2 watercolor paper with 8B pencils, and its efficiency was compared to the efficiency of a commercially available screen-printed carbon electrode. Square wave voltammetry was used for LSD analysis in aqueous medium containing 0.05 mol/L LiClO4 . The limits of detection and quantification were 0.38 and 1.27 µmol/L, respectively. Both electrodes exhibited a similar voltammetric response, which was also confirmed during analysis of a seized LSD sample, with recovery of less than 10%. The seized samples were previously analyzed by GCMS technique, employing the full scan spectra against the software spectral library. The electrode selectivity was also tested against 3,4-methylenedioxymethamphetamine (MDMA) and methamphetamine. It was possible to differentiate these compounds from LSD, indicating that the developed paper-based device has potential application in forensic chemistry analyses.

[Identification and Analysis of LSD Derivatives in Illegal Products as Paper Sheet].

To prevent the abuse of new psychoactive substances (NPS), a total of 2372 substances and two plants are controlled as "Designated Substances" in Japan as of September 2019. Although the distribution of these substances has decreased for the past three years, newly-emerged NPS are still being found. In this study, we detected four lysergic acid diethylamide (LSD) derivatives as designer drugs from four paper sheet products, which were obtained from 2014 to 2017 in Japan. The compounds were identified as 4-Acetyl-N,N-diethyl-7-methyl-4,6,6a,7,8,9-hexahydroindolo[4,3-fg]quinoline-9-carboxamide (ALD-52), N,N,7-triethyl-4,6,6a,7,8,9-hexahydroindolo[4,3-fg]quinoline-9-carboxamide (ETH-LAD), 7-Allyl-N,N-diethyl-4,6,6a,7,8,9-hexahydroindolo[4,3-fg]quinoline-9-carboxamide (AL-LAD), N,N-diethyl-7-methyl-4-propionyl-4,6,6a,7,8,9-hexahydroindolo[4,3-fg]quinoline-9-carboxamide (1P-LSD), by GC-MS, LC-MS, LC-Q-TOF-MS and NMR analyses. Further, we studied the extraction methods of LSD derivatives from paper sheet, and the analytical conditions of GC-MS, LC-MS and LC-FL(fluorescence). Among LSD derivatives, 1P-LSD have been controlled as designated substances (Shitei Yakubutsu) under the Pharmaceutical and Medical Device Act in Japan since April 2016. For the legislation of the other derivatives identified in this study, the evaluation of their pharmacological properties are now in progress.

New psychoactive substances (NPS) prevalence over LSD in blotter seized in State of Santa Catarina, Brazil: A six-year retrospective study.

Designer drugs or new psychoactive substances (NPS) are a heterogeneous group of substances obtained through the modification of chemical structure of some natural products or drugs. NPS illegally commercialized in blotter papers mimicking the most common form of LSD consumption, with a great variability of colours and symbols, have largely increased worldwide, including in Brazil, becoming an important emerging public health issue. In this study, we have evaluated the presence and profile of NPS in blotters seized in the State of Santa Catarina, Brazil, over the period of 2011 to 2017. The state government criminal forensics staff has performed gas chromatography-mass spectrometer (GC-MS) analyses in order to determine the chemical composition of the blotters. During the evaluated period, there was a considerable increase in the seizing of blotters events, from 87 in 2011, to 301 in 2016 and reaching 277 in 2017. There was also an increase in the number of blotters seized per event. Interestingly, while in 2011, 100% of blotters contained LSD, this number decreased to 0,1% in 2014, and achieved 17,6% in 2017, when up to 25 different substances were detected in blotters seized. Drugs such as DOx, NBOMe, fentanyl, mescaline derivatives, triptamines, cathinones, and synthetic cannabinoids were detected and became the major substances found in blotters. In some cases, more than one substance was found in the same blotter, characterizing a new mixture scenario. The presence of several new psychoactive substances in blotters is a reality in forensic toxicology. In Brazil, it might be related to the fact that most of these substances were not considered illegal by Brazilian legislation by the time they emerged.

Psychedelic Microdosing: A Subreddit Analysis.

Self-administration of very low doses of psychedelic drugs to improve mental health and wellbeing and enhance cognitive function, known as microdosing, has received recent media attention, but little research has been conducted. We conducted a content analysis of discussions about microdosing from the online forum Reddit. We examined motivations, dosing practices, and perceived benefits and limitations of microdosing. Motivations included self-management of mental health issues, improvement of psychosocial wellbeing, and cognitive enhancement. Self-reported benefits included cognitive and creative enhancement, reduced depression and anxiety, enhanced self-insight and mindfulness, improved mood and attitude toward life, improved habits and health behaviors, and improved social interactions and interpersonal connections. Perceived limitations included issues related to dosing, adverse physical effects, taking illegal substances, limited or no mental health or cognitive improvement, increased anxiety, unpleasant "off" days, only short-term benefits, and concerns about dependence and drug-related risks. Standard doses of psychedelic drugs provided in therapeutic settings have potential as novel treatments for some mental health conditions, but clinical research is needed to understand if this is also the case for microdosing. In the meantime, harm reduction resources should be developed and made available to provide the best available information on the safer use of self-administered psychedelics.

Lab-made solid phase microextraction phases for off line extraction and direct mass spectrometry analysis: Evaluating the extraction parameters.

The analyses of drugs and metabolites in complex matrices have been widely studied in recent years. However, due to high levels endogenous compounds and matrix complexity, these analyses require a sample pre-treatment step. To this aim, two lab-made extractive phases were integrated to probe electrospray ionization mass spectrometry (PESI-MS) technique for direct analysis of illicit drugs in biological fluids and phorbol esters in Jatropha curcas extract. The polypyrrole (PPy) phase was electropolymerized onto a platinum wire surface by cyclic voltammetry. The molecularly imprinted polymer (MIP) was synthesized and adhered onto a stainless-steel needle with epoxy resin. The PPy-PESI-MS method showed to be linear in a concentration range from 1 to 500 µg L-1, with accuracy values between -2.1 and 14%, and precision values between 0.8 and 10.8%. The MIP-PESI-MS method showed to be linear in a concentration range from 0.9 to 30 mg L-1, with accuracy values between -1.6 and -15.3%, and precision values between 4.1 and 13.5%.

Return of the lysergamides. Part IV: Analytical and pharmacological characterization of lysergic acid morpholide (LSM-775).

Lysergic acid diethylamide (LSD) is perhaps one of the best-known psychoactive substances and many structural modifications of this prototypical lysergamide have been investigated. Several lysergamides were recently encountered as 'research chemicals' or new psychoactive substances (NPS). Although lysergic acid morpholide (LSM-775) appeared on the NPS market in 2013, there is disagreement in the literature regarding the potency and psychoactive properties of LSM-775 in humans. The present investigation attempts to address the gap of information that exists regarding the analytical profile and pharmacological effects of LSM-775. A powdered sample of LSM-775 was characterized by X-ray crystallography, nuclear magnetic resonance spectroscopy (NMR), gas chromatography mass spectrometry (GC-MS), high mass accuracy electrospray MS/MS, high performance liquid chromatography (HPLC) diode array detection, HPLC quadrupole MS, and GC solid-state infrared analysis. Screening for receptor affinity and functional efficacy revealed that LSM-775 acts as a nonselective agonist at 5-HT1A and 5-HT2A receptors. Head twitch studies were conducted in C57BL/6J mice to determine whether LSM-775 activates 5-HT2A receptors and produces hallucinogen-like effects in vivo. LSM-775 did not induce the head twitch response unless 5-HT1A receptors were blocked by pretreatment with the antagonist WAY-100,635 (1 mg/kg, subcutaneous). These findings suggest that 5-HT1A activation by LSM-775 masks its ability to induce the head twitch response, which is potentially consistent with reports in the literature indicating that LSM-775 is only capable of producing weak LSD-like effects in humans.

Advantages of analyzing postmortem brain samples in routine forensic drug screening-Case series of three non-natural deaths tested positive for lysergic acid diethylamide (LSD).

Three case reports are presented, including autopsy findings and toxicological screening results, which were tested positive for the potent hallucinogenic drug lysergic acid diethylamide (LSD). LSD and its main metabolites were quantified in brain tissue and femoral blood, and furthermore hematoma and urine when available. LSD, its main metabolite 2-oxo-3-hydroxy-LSD (oxo-HO-LSD), and iso-LSD were quantified in biological samples according to a previously published procedure involving liquid-liquid extraction and ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). LSD was measured in the brain tissue of all presented cases at a concentration level from 0.34-10.8µg/kg. The concentration level in the target organ was higher than in peripheral blood. Additional psychoactive compounds were quantified in blood and brain tissue, though all below toxic concentration levels. The cause of death in case 1 was collision-induced brain injury, while it was drowning in case 2 and 3 and thus not drug intoxication. However, the toxicological findings could help explain the decedent's inability to cope with brain injury or drowning incidents. The presented findings could help establish reference concentrations in brain samples and assist in interpretation of results from forensic drug screening in brain tissue. This is to the author's knowledge the first report of LSD, iso-LSD, and oxo-HO-LSD measured in brain tissue samples.

The detection and prevention of unintentional consumption of DOx and 25x-NBOMe at Portugal's Boom Festival.

OBJECTIVE: This paper describes the misrepresentation of LSD at Portugal's Boom Festival 2014 and the prevention of unintentional consumption of DOx and 25x-NBOMe among LSD consumers attending a drug-checking service. METHODS: Two hundred forty-five drug samples expected to contain LSD were submitted to the drug-checking service for chemical analysis. One hundred ten post-test questionnaires were successfully matched with test results. RESULTS: About 67.3% of the alleged LSD samples tested contained only LSD; 0.8% contained LSD combined with adulterants; 24.1% did not contain LSD but did contain another psychoactive substance, including 11.4% that were 2,5-dimethoxyamphetamine derivatives and 9.8% that were N-benzyl-2,5-dimethoxyphenethylamine derivatives; and no psychoactive substance was detected in 7.8%. The majority of service users who received unexpected test results regarding their alleged LSD (74.2%) reported that they did not intend to consume the drug. Following dissemination of alerts on day 2, a larger than expected proportion of all tests conducted were for LSD, when comparing the 2014 festival to 2012, where no such alert was disseminated. CONCLUSIONS: Although these results support the provision of integrated drug-checking services in party settings, evidence of their utility and effectiveness would be improved through future research incorporating more robust measures of outcomes following provision of drug-checking results.

LSD Detection and Interpretation in Hair.

Lysergic acid diethylamide (LSD) is a powerful hallucinogen, active at very low dosages, with, as a direct consequence, potential difficulties to be detected and quantified in a clinical or forensic context, in body fluids and even more in hair. The aim of this work is to review literature data related to hair analysis of LSD with a particular focus on the main issues encountered in LSD detection in hair. Results of LSD investigation in hair remain difficult to interpret regarding the very sparse data available on LSD concentrations in hair (n=10). The possibility of pubic hair contamination by urine, as well as the lack of data about LSD incorporation and stability in pubic and head hair, further challenges the interpretation of negative or positive results. The absence of LSD in head hair should be carefully considered, as it does not formally exclude LSD consumption. In all cases of positive results, the interpretation of LSD concentrations in hair remains uncertain and it seems utopian to distinguish repeated intake from single exposure using LSD hair concentration values. Furthermore, a positive result in pubic hair cannot be used to formally prove repeated use of LSD, even in the case of a documented recent use of LSD.

Lysergic acid amide as chemical marker for the total ergot alkaloids in rye flour - Determination by high-performance thin-layer chromatography-fluorescence detection.

Ergot alkaloids are generally determined by high-performance liquid chromatography (HPLC) coupled to fluorescence detection (FLD) or mass selective detection, analyzing the individual compounds. However, fast and easy screening methods for the determination of the total ergot alkaloid content are more suitable, since for monitoring only the sum of the alkaloids is relevant. The herein presented screening uses lysergic acid amide (LSA) as chemical marker, formed from ergopeptine alkaloids, and ergometrine for the determination of the total ergot alkaloids in rye with high-performance thin-layer chromatography-fluorescence detection (HPTLC-FLD). An ammonium acetate buffered extraction step was followed by liquid-liquid partition for clean-up before the ergopeptine alkaloids were selectively transformed to LSA and analyzed by HPTLC-FLD on silica gel with isopropyl acetate/methanol/water/25% ammonium hydroxide solution (80:10:3.8:1.1, v/v/v/v) as the mobile phase. The enhanced native fluorescence of LSA and unaffected ergometrine was used for quantitation without any interfering matrix. Limits of detection and quantitation were 8 and 26µg LSA/kg rye, which enables the determination of the total ergot alkaloids far below the applied quality criterion limit for rye. Close to 100% recoveries for different rye flours at relevant spiking levels were obtained. Thus, reliable results were guaranteed, and the fast and efficient screening for the total ergot alkaloids in rye offers a rapid alternative to the HPLC analysis of the individual compounds.

Return of the lysergamides. Part III: Analytical characterization of N6 -ethyl-6-norlysergic acid diethylamide (ETH-LAD) and 1-propionyl ETH-LAD (1P-ETH-LAD).

The psychoactive properties of lysergic acid diethylamide (LSD) have fascinated scientists across disciplines and the exploration of other analogues and derivatives has been motivated by deepening the understanding of ligand-receptor interactions at the molecular level as well as by the search for new therapeutics. Several LSD congeners have appeared on the new psychoactive substances (NPS) market in the form of blotters or powders. Examples include 1-propionyl-LSD (1P-LSD), AL-LAD, and LSZ. The absence of analytical data for novel compounds is a frequent challenge encountered in clinical and toxicological investigations. Two newly emerging lysergamides, namely N6 -ethyl-6-norlysergic acid diethylamide (ETH-LAD) and 1P-ETH-LAD, were characterized by gas chromatography-mass spectrometry (GC-MS), low and high mass accuracy electrospray MS(/MS), GC solid-state infrared analysis, high performance liquid chromatography diode array detection as well as nuclear magnetic resonance spectroscopy. Limited analytical data for ETH-LAD were previously available, whereas information about 1P-ETH-LAD has not previously been encountered in the scientific literature. This study extends the characterization of lysergamides distributed on the NPS market, which will help to make analytical data available to clinicians, toxicologists, and other stakeholders who are likely to encounter these substances. The analysis of a test incubation of 1P-ETH-LAD with human serum at 37°C by LC single quadrupole MS at various time points (0-6 h, once per hour and one measurement after 24 h) revealed the formation of ETH-LAD, suggesting that 1P-ETH-LAD might serve as a pro-drug. 1P-ETH-LAD was still detectable in serum after 24 h. Copyright © 2017 John Wiley & Sons, Ltd.

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

Ultrasensitive analysis of lysergic acid diethylamide and its C-8 isomer in hair by capillary zone electrophoresis in combination with a stacking technique and laser induced fluorescence detection.

This article deals with the development and validation of a novel capillary zone electrophoresis (CZE) with laser induced fluorescence detection method for the analysis of lysergic acid diethylamide (LSD) and its isomer iso-LSD in hair samples. The separation of both analytes has been achieved in less than 13 min in a 72-cm effective length capillary with 75-µm internal diameter. As running buffer 25 mM citrate, pH 6.0 has been employed and separation temperature and voltage of 20 °C and 13 kV respectively, were applied. Field amplified sample injection (FASI) has been employed for on-line sample preconcentration, using ultrapure water containing 117 µM H3PO4 as optimum injection medium. Injection voltage and time have been optimized by means of experimental design, obtaining values of 7 kV and 15s, respectively. Methylergonovine has been employed as internal standard in order to compensate irreproducibility from electrokinetic injection. The analytical method has been applied to hair samples, previous extraction of the target analytes by ultrasound assisted solid-liquid extraction at 40 °C for 2.5 h, employing acetonitrile as extracting solvent. Linear responses were found for LSD and iso-LSD in matrix-matched calibrations from around 0.400 up to 50.0 pg mg(-1). LODs (3 S/N) in the order of 0.100 pg mg(-1) were calculated for both analytes, obtaining satisfactory recovery percentages for this kind of sample.

Analysis of psilocin, bufotenine and LSD in hair.

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.