Detection Of Lysergic Acid Diethylamide Research Articles

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.

Enhanced detection of lysergic acid diethylamide using Ehrlich reagent and screen-printed electrodes: A hybrid method for application in forensic analysis

In forensic investigations, the presumptive identification of illicit substances, such as Lysergic Acid Diethylamide (LSD), is crucial. While the Ehrlich's colorimetric reagent (EHR) is commonly employed for LSD detection, producing a characteristic colour change, its lack of selectivity often leads to false-positive or misinterpreted results. Addressing this, we propose a novel method combining electrochemical detection with EHR, enhancing selectivity for LSD’s preliminary identification in forensic samples. This method utilizes a screen-printed carbon electrode (carbon-SPE) in a pH 12 phosphate buffer. We observed two irreversible oxidation processes for LSD at Epa= + 0.35 V (Ox1) and + 0.65 V (Ox2), and for EHR at + 0.62 V and + 0.83 V (vs Ag/AgCl). The LSD + EHR combination displayed three distinct irreversible oxidation processes at + 0.35 V, + 0.66 V, and + 0.86 V. This approach provides three analytical responses for LSD identification: (1) colour change post-EHR test; (2) voltammetric detection of LSD’s two oxidation processes on carbon-SPE; (3) decreased peak current of LSD at Ox1 post-reaction after EHR. Additionally, our method facilitates LSD quantification, exhibiting a low limit of detection (LOD) of 0.69 μmol/L, and consistent electrochemical responses (RSD < 3.0 %) using the same or different carbon-SPEs. Interference studies with other illicit drugs underscored the method’s reliability and selectivity in LSD detection. Moreover, addition-recovery studies on real seized samples approached 100 %, and LSD identification was corroborated by QTOF-LC/MS analyses. Therefore, combining voltammetry with carbon-SPE and EHR offers significant potential for a rapid, simple, and selective LSD screening test in forensic analysis.

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.

Concentrations of LSD, 2-oxo-3-hydroxy-LSD, and iso-LSD in hair segments of 18 drug abusers

Lysergic acid diethylamide (LSD) is one of the most widely abused hallucinogens, which can alter consciousness, produce mental disorder, and cause harmful behavior. 1-Propionyl-LSD (1 P-LSD), a novel derivative of LSD, has the similar hallucinogenic effect. It is a control substance in several countries. 1 P-LSD can act as a prodrug for LSD and is rapidly hydrolyzed to LSD in humans. Therefore, LSD use should be confirmed by the absence of 1 P-LSD and in the detection of LSD. Here, we describe a LC–MS/MS method for the simultaneous extraction of LSD, iso-LSD, 2-oxo-3-hydroxy-LSD, and 1 P-LSD from hair. Hair samples (25 mg) were pulverized by cryogenic grinding in methanol. The limits of detection were 0.2–1 pg/mg and the limits of quantification were 0.5–2 pg/mg. This method was validated and applied to hair samples from 18 suspects who may have used LSD. Segmental hair analysis revealed a decrease in the LSD concentrations from the proximal to the distill end, while 1 P-LSD was not detected in any hair segments. The interpretation of hair analysis results of LSD still remains difficult. Nevertheless, concentrations of LSD and iso-LSD in human hair from 18 LSD users were reported. LSD concentrations were from <LOQ to 4.0 pg/mg (n = 18, median 1.5 pg/mg) in the proximal 0–3 cm segment, from <LOQ to 1.8 pg/mg (n = 8) in the 3–6 cm segment, and from <LOQ to 0.6 pg/mg (n = 4) in the 6–9 cm segment. Iso-LSD ranged from <LOQ to 1.4 pg/mg (n = 4) in the 0–3 cm segment and was detectable only in one 3–6 cm segment. To our knowledge, this is the first study to monitor LSD together with 1 P-LSD in hair.

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.

Rapid and simple voltammetric screening method for Lysergic Acid Diethylamide (LSD) detection in seized samples using a boron-doped diamond electrode

We present a new approach for the screening method of Lysergic Acid Diethylamide (LSD) in blotter papers using square wave voltammetry with a Boron-Doped Diamond Electrode (BDDE). The LSD electrochemical detection is based on an oxidation process at the BDDE in 0.1 mol L−1 acetate buffer pH 4.0. The BDDE exhibited a highly stable response for LSD oxidation (peak current and peak potential) with a relative standard deviation lower than 1.6 % (N = 10). The linear range for LSD determination spans over two orders of magnitude (5.0–100 μmol L−1) with an excellent linear regression coefficient (r2 > 0.999) and a LOD of 0.5 μmol L−1, which is sufficiently low to detect this drug in seized samples. An interference study for LSD detection in seized blotter papers was performed for twenty (20) synthetic drugs belonging to the phenethylamines derivative groups. The analytical performance of the proposed approach revealed itself as an easy, rapid, and selective screening method for the detection of LSD in blotter papers and other presentation formats.

Simple and Fast Analysis of LSD by Cyclic Voltammetry in Aqueous Medium

The application of electrochemical analysis within the forensic scenario has been widely explored, mainly in the context of the analysis of illicit drugs. In this regard, voltammetric measurements are particularly sensitive and specific. Psychedelic LSD (lysergic acid diethylamide) appears in seized blotters, and its apprehension is constant on a global scale. In this study, we have developed a simple, fast, and sensitive voltammetric method to quantify LSD by using a glassy carbon electrode. The use of an aqueous solution of KClO4 as supporting electrolyte has allowed us to design a less polluting methodology. Concerning the developed method, the anodic peak observed at 0.88 V vs. Ag/AgCl is proportional to the concentration of LSD. The limits of detection and quantification of the method are 0.987 and 3,29 µmol L-1, respectively, which enables detection of LSD at a concentration level of µg per mL of the extraction solution. The same method can also be employed to detect 25H-NBOMe, a compound belonging to the class of NBOMes, which exert practically the same psychoactive effect as LSD.

Immunochemical extraction and detection of LSD in whole blood

Polyclonal antibodies raised against the hallucinogenic drug, lysergic acid diethylamide (LSD), were used to detect and extract drug from whole blood samples. An indirect ELISA was used to detect as little as 1 pg of total drug in 25 μl blood. The limit of detection of the immunoassay, calculated from the mean−3 SD was 39 pg/ml. The analytical recovery of LSD (2.5–0.2 ng/ml) from whole blood was 102–113%. Within-run CVs for LSD spiked in blood at 1.25, 0.16 and 0.04 ng/ml were 5.6, 3.1, and 8.9%, respectively ( n=4). There was an overall decrease in precision when whole blood was used in place of urine, due to the increased complexity of the matrix. However, using this technique LSD was calibrated in blood in the sub-ng/ml region of forensic interest. Immunoaffinity extraction was used to isolate LSD from blood and urine samples. The affinity support was prepared by covalently attaching anti-LSD antibodies to Protein A-coated agarose beads. No pre-treatment of the sample was required other than the addition of neutral buffer. Sub-ng/ml concentrations of LSD were routinely extracted from blood and urine samples with greater than 80% recovery of drug. This technique, which could be used to extract LSD from blood and urine samples prior to confirmatory drug analysis, could be completed in about 10 min.

New synthesis and characterization of (+)-lysergic acid diethylamide (LSD) derivatives and the development of a microparticle-based immunoassay for the detection of LSD and its metabolites.

In this paper are reported the synthesis and characterization of three LSD derivatives. On the basis of several analytical characterization studies, the most stable derivative has been selected and a procedure to covalently link the derivative to polystyrene microparticles through a carrier protein has been developed. In addition, two new LSD immunogens have been synthesized and characterized, and from these immunogens antibodies that recognize not only LSD but also several major LSD metabolites have been generated. Using the selected derivative and antibody, a homogeneous microparticle-based immunoassay has been developed for the detection of LSD in human urine with the required sensitivity and specificity for an effective screening assay. The performance of this LSD OnLine assay has been evaluated using the criteria of precision, cross-reactivity, correlation to the Abuscreen LSD RIA and GC/MS/MS, assay specificity, and limit of detection.

Detection of LSD and metabolite in rat hair and human hair.

To examine the feasibility of detecting lysergic acid diethylamide (LSD) and its metabolites in hair, LSD was administered to rats with pigmented hair at 0.05, 0.1, 0.5, 1, and 2 mg/kg intraperitoneally once per day for 10 successive days. The rats were shaved just before the first administration, and newly grown hair was collected 4 weeks later. After being washed with 0.1% sodium dodecyl sulfonate and water and being dried in a desiccator, each 20-mg hair sample was extracted with 2 mliter methanol-5N HCl (20:1) under ultrasonication for 1 h and stored at room temperature for 14 h. The extract was evaporated to dryness, extracted from 0.1M NaOH with dichloromethane, and derivatized with a mixture of trimethylsilylimidazole, bis-(trimethylsilyl)acetamide, and trimethylchlorosilane (3:3:2, v/v/v) for gas chromatographic-mass spectrometric (GC-MS) analysis using LSD-d10 or lysergic acid methylpropylamide (LAMPA) as the internal standard. Selected ions were monitored at m/z 395, 293, and 279 for TMS-LSD and at m/z 381, 279, and 254 for the trimethylsilyl derivative of N-demethyl-LSD (TMS-norLSD). LSD and norLSD were also detected by high-performance liquid chromatography (HPLC) with fluorometric detection (excitation, 315 nm; emission, 420 nm). LSD was detected in the rat hair following the lowest dose (0.05 mg/kg), whereas norLSD was only detectable in the hair following the highest dose (2 mg/kg). The same GC-MS and HPLC assays were applied to the analysis of hair from 17 self-reported LSD users, and LSD was detected in two of the samples.

Detection of lysergic acid diethylamide, Δ 9-tetrahydrocannabinol and related compounds by plasma chromatography

Plasma chromatography as a method for ultratrace qualitative and quantitative detection of organic compounds is especially well suited for detection of gas chromatographic effluents. The optimum range of sample quantity is 10 −6 to 10 −12 g for detection and identification of a compound by use of its characteristic positive and negative mobility spectra. The type of reference mobility spectra produced by alkanes, aromatics, esters, halogenated compounds, nitrogenated compounds and organic acids have been previously reported. This study presents the reference mobility spectra produced for lysergic acid diethylamide (LSD), Δ 9-tetrahydrocannabinol (Δ 9-THC), digitoxigenin and several biochemical compounds of research significance. LSD and Δ 9-THC in a mixture can be detected and identified by plasma chromatography positive mobility spectra in quantities of 10 −7 g or less. All the compounds investigated in this study display strong MH + ions along with other ions primarily of the type (M)NO +, (M) 2H +. None of these compounds exhibits negative mobility spectra.

A rapid screening procedure for some “street drugs” by thin-layer chromatography

The extraction of some illicit drugs with 95% ethanol and subsequent analysis on pre-coated thin layers of silica gel (E. Merck) made the tentative identification of some constituents of “street drugs” 1 1 The term “Street Drugs” refers to both legally and illegally manufactured drugs that are sold in the illicit street market and usually are of unknown composition. possible. Two detecting reagents were used, p-dimethylaminobenzaldehyde and iodoplatinate. p-Dimethylaminobenzaldehyde was used for the detection of lysergic acid diethylamide, psilocybin, monomethyltryptamine, dimethyltryptamine, and iodoplatinate for strychnine, mescaline, methamphetamine, amphetamine, phencyclidine. The thin-layer chromatograms derived characteristics of lysergic acid diethylamide and phencyclidine were unique, allowing for the relatively easy detection of these two compounds. The procedure is most useful for the rapid screening of illicit drugs for the presence or absence of the listed compounds. The unequivocal identity of these compounds is not established, but the procedure does permit tentative identification.