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Pepper sprays of the OC type constitute the majority of self-defense sprays available on the market. The active ingredient in these preparations is pepper extract: Oleoresin Capsicum, which contains capsaicinoids - natural compounds with irritant properties. Preparations from OC pepper sprays can be distinguished based on differences in the quantitative ratios of four main capsaicinoids: capsaicin, dihydrocapsaicin, nordihydrocapsaicin, and nonivamide. This raises the question whether information on the quantitative ratios of capsaicinoids can also provide answers to questions regarding comparisons of traces of OC preparations, such as whether traces revealed on the clothing of the victim could originate from an OC spray secured from the suspect, or whether traces on the clothing of the suspect and the victim could come from the same pepper spray. Such comparisons would be viable only if the capsaicinoid profile remained unchanged during evidence storage and as a result of solvent extraction from the tested material. The aim of the presented research was to determine if this is indeed the case. Model aging experiments were conducted to examine whether the capsaicinoid profile in traces of OC preparations changed over time and whether solvent extraction affected this profile. Samples of five different OC preparations were applied to cotton swabs, which, after the evaporation of volatile solvents, were placed in three types of packaging with varying levels of tightness and transparency (tight amber vials, polyethylene bags, paper envelopes). These prepared samples underwent solvent extraction with methanol and analysis using gas chromatography – mass spectrometry, after 28, 84, 147, 196, 252, and 301 days from preparation. The likelihood ratio (LR) was applied as a statistical tool to investigate the data obtained. The LR model was computed using the three variables based on the relative content of nordihydrocapsaicin, nonivamide, and dihydrocapsaicin. The cotton swabs used in the experiments served as a model for both the swabs used by the police for securing liquid evidence and the cotton clothing of individuals sprayed with OC pepper sprays. The findings of the conducted studies suggest that the quantitative relationships of capsaicinoids indeed change over time, both in preparations stored in original containers and in traces of these preparations present on clothing. For traces of OC preparations secured on swabs or present on clothing, these changes are more significant the longer the sample is stored and the less airtight the packaging used. [Display omitted] • Pepper sprays differ in the quantitative ratios of capsaicinoids. • The capsaicinoid profile in traces, e.g., on clothing, changes over time. • Changes depend on the storage duration and packaging method of the samples. • Changes are more significant with longer storage time and less airtight packaging. • Comparing capsaicinoid profiles in traces and preparations is not advisable. [ABSTRACT FROM AUTHOR]

F-500 Encapsulator Agent (EA) is a fire suppression agent that is an alternative to traditional firefighting foams. It is marketed as having the capability to act on all four parts of the fire tetrahedron as well as being environmentally friendly and non-toxic. An internal survey of the use of F-500 EA by fire departments encountered by the Bureau of Alcohol, Tobacco, Firearms and Explosives (ATF) ignitable liquid detection canine (ILDC) handlers in 2022 showed that this product is not yet in widespread use across the country, but where it has been implemented, it is frequently utilized on a variety of types of fires. Additional agencies are researching the product to determine if it should be adopted. As this product appears to be growing in popularity, it is important to understand whether the use of the product would affect a canine's ability to detect ignitable liquids or a forensic laboratory's ability to identify the presence of an ignitable liquid. Burned wood and burned carpet, two commonly encountered substrates, were spiked with gasoline or a heavy petroleum distillate (HPD) and F-500 EA was applied. At various time intervals, ILDC teams surveyed the samples and laboratory analysis was conducted. Results showed that the presence of F-500 EA can negatively affect canine alerts and the laboratory's ability to identify ignitable liquids. • F-500 Encapsulator Agent appears in data during routine ignitable liquid analysis with passive headspace concentration. • The effect of the product on canine detection and ignitable liquid analysis varied based on substrate and ignitable liquid. • Results show the product has the potential to interfere with canine detection of ignitable liquids and laboratory analysis. [ABSTRACT FROM AUTHOR]

Drug-related fatalities in the EU are predominantly associated with opioids. MDMA (Ecstasy) consumption results in fewer lethal intoxications despite its widespread use. This study investigates MDMA-related fatalities, focusing on enantiomer ratios of MDMA and its metabolite MDA to explore the role of metabolism in fatal outcomes. MDMA induces euphoria, increased empathy, and physiological effects such as tachycardia, hypertension, and hyperthermia. Metabolism mainly involves CYP1A2 and CYP2D6, with polymorphism of the latter influencing metabolism rates. Our institute observed several MDMA-related fatalities, which prompted an investigation into the potential role of inefficient drug metabolism in these cases. A novel quantitative chiral analysis method was developed and validated for MDMA, MDA, amphetamine and methamphetamine enantiomers in human blood. Analysis of post mortem blood samples from eleven MDMA-related fatalities exhibited a wide range of concentrations and enantiomer ratios. Variability in R/S MDMA ratios, however, could be linked to the time period of metabolism. Hair analysis revealed high MDMA concentrations in all segments, irrespective of prior drug abuse anamnesis. Therefore, hair analysis may not be suitable for the assessment of past drug use in ecstasy-related fatalities. The results indicated that elevated levels of the MDMA enantiomer are correlated with longer survival times in cases of intoxication. However, there was no clear evidence for slowed MDMA metabolism as a cause of lethal intoxications. While challenges remain due to the diversity of cases, this study contributes valuable insights into ecstasy intoxications, aiding future interpretation of post mortem analysis., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 The Authors. Published by Elsevier B.V. All rights reserved.)

Background: Post-mortem toxicology constantly deals with the research of reliable alternative matrices to be applied in case of highly damaged corpses (such us carbonized, skeletonized, human remains, etc.). Teeth represent a promising alternative matrix since dental tissues are endowed by different features, resistance and stability after death., Scope: Since scant literature reported on the pharmacokinetics and mechanism of incorporation of xenobiotics into dental tissues, this pilot research aims to investigate whether in the pulp can be detected the same substances found in blood in drug related death cases. Secondly, the study is addressed to disclose the possible deposit of drugs in dental hard tissues (dentine and/or enamel), thus contributing to reconstruct the drug abuse history (timing, e.g.)., Materials and Methods: The study experimented with a novel method to separately analyse dental enamel, dentin, and pulp, applied to 10 teeth collected during autopsies of drug-related deaths along with blood and hair samples for classic toxicological analyses. Each tooth was prepared by "pulverization technique" and then analysed by gas chromatography paired with mass spectrometry (GC-MS) and ultra high performance liquid chromatography coupled to high resolution mass spectrometry (UHPLC/HR-MS) for searching cocaine, opiates, and metabolites. The results were then compared with those obtained from blood and hair samples., Results: Preliminary results demonstrated that teeth differ from any other classic matrix (blood and hairs) since the qualitative correspondence of the detected substances between pulp and blood as well as dental hard tissues and hair suggests that they can be useful in post-mortem evaluation as a unique matrix for both acute and chronic assumptions of drugs. The mechanism of accumulation of substances in mineralized dental tissues emerged the most significant result, being influenced by the type of molecule and the method of assumption. The main limitation of this study is the limited availability of the sample and the absence of anamnestic information of the time, rates and method of drug assumption during life. Further research is necessary to systematically investigate the distribution of different substances within the different tissues of the tooth., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 The Authors. Published by Elsevier B.V. All rights reserved.)

Drug use is prevalent in prisons with drugs associated with depressant effects found to be more prevalent than stimulants. Synthetic cathinones (SCats; often sold as "bath salts", "ecstasy", "molly", and "monkey dust") are the second largest category of new psychoactive substances (NPS) currently monitored by the European Monitoring Centre for Drugs and Drug Addiction (EMCDDA) and are commonly used as substitutes for regulated stimulants, such as amphetamine, cocaine, and MDMA. N,N-dimethylpentylone (also known as dimethylpentylone, dipentylone, and bk-DMBDP) was detected for the first time in the Scottish prisons in seven powder samples seized between January and July 2023. Samples were analyzed using gas chromatography-mass spectrometry (GC-MS), ultra-high performance liquid chromatography-quadrupole time of flight mass spectrometry (UPLC-QToF-MS), and nuclear magnetic resonance imaging (NMR). Dimethylpentylone was detected alongside other drugs in four samples, including the novel benzodiazepine desalkylgidazepam (bromonordiazepam) and the synthetic cannabinoid receptor agonists (SCRAs) MDMB-INACA and MDMB-4en-PINACA., Competing Interests: Declaration of Competing Interest None, (Copyright © 2024 The Authors. Published by Elsevier B.V. All rights reserved.)

Background: With the decline of the use of ketamine, one of the common drugs of abuse in Hong Kong, detection of ketamine-related analogues in local laboratories has been encountered., Aim: A brief account of the occurrence of fluorodeschloroketamine (FDCK) in forensic cases is reported through a retrospective study of all drug seizures and driving under the influence of drugs (DUID) cases since its first appearance., Methods: Identification of FDCK in drug seizures was achieved through gas chromatography - mass spectrometry (GC-MS) and/or liquid chromatography - diode array detection (LC-DAD) methods while its quantification was performed using gas chromatography - flame ionization detection (GC-FID). For the analysis of blood samples in DUID cases, identification and quantification were performed using LC-MS/MS by monitoring the respective transitions of FDCK and fluorodeschloronorketamine (FDCNK) using ketamine-d 4 and norketamine-d 4 respectively as internal standards., Results: Since its first submission in November 2018, a total of 74 drug seizure cases (151 items) and 6 drug driving cases were encountered till December 2019. Drug seizures found with FDCK were physically similar to those of ketamine seizures. The majority of items were detected with FDCK only (103 items, ∼67%) or as a mixture of FDCK with ketamine (42 items, ∼28%). The drug purity detected with either FDCK only or FDCK mixed with ketamine was high which was similar to those purity found in ketamine seizures. The blood drug concentrations of FDCK of the 6 drug driving cases were in the range of <0.002-1.1 μg/mL and other psychoactive drug(s)/metabolite(s) were also identified. Except for one case where the analysis of the metabolite, fluorodeschloronorketamine (FDCNK), was not conducted due to insufficient sample, the FDCK (FDCNK) concentrations in blood found in the 6 cases were <0.002 (0.005), 0.002 (0.002), 0.002 (0.003), 0.02 (0.035), 0.87 (0.44) and 1.1 (not determined) μg/mL., Conclusions: With the drug seizures found with FDCK resembled in physical appearance with ketamine seizures, users might likely misuse it as ketamine. Though complicated by other drugs found, it is speculated that the two cases with higher concentration of FDCK found in blood (1.1 and 0.87 μg/mL) might have contributed to the impairment observed., Competing Interests: Declaration of Competing Interest The authors declare that they have no known financial or personal interest that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

Wastewater based epidemiology (WBE) has been used worldwide to estimate drug consumption routinely. Even though WBE provides valuable data to support legal and health interventions associated to drug use, monitoring studies in Portuguese wastewaters are scarce. Hence, this work aimed to estimate the consumption of some conventional abuse and illicit drugs such as amphetamine (AMP), methamphetamine (MAMP), 3,4-methylenedioxymethamphetamine (MDMA), and the synthetic cathinones buphedrone (BPD), butylone (BTL), 3,4-dimethylmethcathinone (3,4-DMMC) and 3-methylmethcathinone (3-MMC), considering not only the liquid phase, but also the suspended particulate matter (SPM). Moreover, the enantiomeric profiling of the samples was studied, exploring for the first time the possible enantioselective sorption of these drugs onto SPM. For that, 24 h composite raw wastewaters were collected from a conventional wastewater treatment plant (WWTP) in Portugal. After extraction, the liquid phase and SPM extracts were derivatized with an enantiomerically pure reagent and then, analysed using a gas chromatography-mass spectrometry (GC-MS) analytical method. The results showed a low and non-enantioselective adsorption to SPM at environmental relevant levels. Only (S)-AMP was detected in two SPM samples, whereas AMP, MAMP, MDMA, BPD, and 3,4-DMMC were detected in the liquid phase. AMP was the most frequently found drug with an estimated load up to 166.0 mg day -1 1000 people -1 and mostly found with enrichment of (S)-AMP. Nevertheless, (R)-AMP was also determined, which may be related to the consumption of either the illicit racemic AMP or the medicine (R)-deprenyl. The use of MDMA, MAMP and synthetic cathinones (BPD and 3,4-DMMC) was also suggested in Portugal. Nevertheless, the levels and the consumption estimate of the target chemicals were lower than in other European countries or worldwide. These findings provide the first step to the implementation of WBE monitoring campaigns to assess the status of drug consumption in Portuguese communities, contributing to the understanding of drug use patterns and trends worldwide and helping enforce preventive measures., Competing Interests: Declaration of Competing Interest The authors declare no conflict of interest., (Copyright © 2024 The Authors. Published by Elsevier B.V. All rights reserved.)

Nitrous oxide (N 2 O), also known as laughing gas, has a euphoric effect and is becoming increasingly popular as a recreational inhalant drug. Deaths caused by recreational nitrous oxide abuse are rare, but may still occur. Although some methods for the quantification of N 2 O by GC-MS have been reported, elimination of carbon dioxide interference and the choice of a suitable internal standard remain current limitations to accurate N 2 O quantification. Here, a validated method using headspace-gas chromatography-mass spectrometry (HS-GC-MS) is described that allows the quantification of N 2 O in human blood samples: sodium hydroxide is used to remove carbon dioxide, and n-pentane is chosen as a suitable internal standard. Collectively, the validation results show a good linear relationship of N 2 O in blood within the concentration range of 0.02 ∼ 0.5 mL/mL and an LOD of 0.005 mL/mL. Subsequent application of the validated method to two real mortality cases due to N 2 O intoxication provided reference values for blood concentrations in forensic cases. Other biological specimens (gaseous samples and tissues) of the deceased were also analyzed to demonstrate that the deaths were caused by asphyxia due to the inhalation of N 2 O., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

The location of human remains is performed primarily through the aid of cadaver detection dogs, which rely on the malodour produced through decomposition of decaying bodies. Malefactors will attempt to conceal these putrefactive odours through chemical additions such as lime, which is also wrongly believed to accelerate decomposition and prevent the identification of the victim. Despite the frequency of lime in forensic applications, to date no research has been performed to determine its effect on the volatile organic compounds (VOCs) released during human decomposition. This research was therefore conducted to ascertain the effects of hydrated lime on the VOC profile of human remains. Two human donors were used in a field trial at the Australian Facility for Taphonomic Experimental Research (AFTER): one donor was covered with hydrated lime, and the other had no chemical additions acting as a control. VOC samples were collected over a period of 100 days and analysed using comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC×GC-TOFMS). The volatile samples were accompanied by visual observations of how decomposition progressed. The results showed that lime application decreased the rate of decomposition and decreased total carrion insect activity. Lime increased the abundance of VOCs during the fresh and bloat stages of decay, however the abundance of compounds plateaued during active and advanced decomposition and were much lower than those detected from the control donor. Despite this suppression of VOCs, the study found that dimethyl disulfide and dimethyl trisulfide, key sulfur-containing compounds, were still produced in high quantities, and can thus still be used to locate chemically altered human remains. Knowledge of the effects of lime on human decomposition can inform the training of cadaver detection dogs, and ensure a greater chance at locating victims of crimes or mass disasters., Competing Interests: Declaration of Competing Interest The authors declare that there are no conflicts of interest., (Copyright © 2023 The Authors. Published by Elsevier B.V. All rights reserved.)

Bones are among the structures most likely to be recovered after death. However, the low quantity of preserved DNA and complex processing from sample to DNA profile make forensic DNA analysis of bones a challenging task. Raman spectroscopy and gas chromatography-mass spectrometry (GC/MS), have the potential to be useful as screening tools for DNA analysis and in decomposition studies. The objective of this research was to assess the usefulness of such molecular investigations. Femur samples collected from 50 decomposing human bodies were subjected to Raman spectroscopy and GC/MS. Assessment of nuclear DNA quantity and short tandem repeat (STR) genotyping efficiency were also performed. Raman parameters (crystallinity, carbonate-to-phosphate ratio, mineral-to-matrix ratio) and detected lipids were recorded. Background fluorescence proved problematic for Raman analysis of forensic bones. Regardless, it was not associated with less preserved DNA or less detected STR alleles. Fatty acids, hydrocarbons, and five types of fatty acid methyl esters (FAMEs) were detected. The main phosphate peak position in Raman spectra was significantly correlated with preserved DNA (p = 0.03713), while significantly more STR alleles were detected in bones containing methyl hexadecenoate (p = 0.04236). Detection of FAMEs in the bone matrix suggests a reaction between methanol produced by bacteria and free fatty acids, which are not associated with the level of preservation of endogenous DNA. The techniques assessed have shown to be useful in molecular taphonomy studies and forensic genetics. • Raman spectroscopy and gas chromatography-mass spectrometry, are useful in decomposition studies. • the main phosphate peak position in Raman spectra was significantly correlated with preserved DNA. • significantly more STR alleles were detected in bones containing methyl hexadecenoate. • bacterial methanol and free fatty acids form esters during decomposition. • Raman analysis of forensic bones can be hampered by background fluorescence. [ABSTRACT FROM AUTHOR]

Analysis of volatile hydrocarbons in blood from fire-related deaths provides useful information such as whether the victim inhaled smoke from the fire before death or whether an accelerant was used in the fire. In this study, we used headspace gas chromatography-mass spectrometry to quantify volatile hydrocarbons in post-mortem heart blood from 121 fire victims. The cases were classified into the following four groups according to the detected volatile hydrocarbons: construction fires without accelerants, kerosene fires, gasoline fires, and a group with no fire-related hydrocarbons detected (other fires). We investigated the relationships between blood concentrations of carboxyhemoglobin (COHb) and volatile hydrocarbons, and between various volatile hydrocarbons. The mean COHb concentrations were higher in the construction fire group than in the kerosene and gasoline fire groups. In the construction fire group, there was a high correlation coefficient between the concentrations of benzene and COHb and relatively high coefficient correlations between the concentrations of benzene and toluene, benzene and xylene, toluene and styrene, and ethylbenzene and styrene. Our results indicate that the relationships between benzene, xylene, and toluene concentrations could be used to distinguish between deaths in construction fires, kerosene fires, and gasoline fires. • Blood volatile hydrocarbons in 121 fire victims were quantified by GC-MS. • The cases were classified into four groups according to the detected hydrocarbons. • The relationships between five hydrocarbons in blood were investigated. • A high ratio of toluene/benzene in blood could indicate a gasoline fire. • Benzene, xylene, and toluene ratios could be used to identify kerosene fire cases. [ABSTRACT FROM AUTHOR]

Introduction: Ketamine is primarily used as an anaesthetic or for analgesics in medical treatment, but due to its dissociative and hallucinogenic effects, abuse has increased in the past years leading to several drug impaired driving cases., Methods: Eight DUID (driving under the influence of drugs) cases involving ketamine from two institutes of legal medicine over a period from January 2021 to January 2023 were evaluated. The cases were compared with regard to psychomotor impairments, adverse effects on driving performance and co-consumption of drugs. Analyses of ketamine were carried out by high performance liquid chromatography with diode array detection (HPLC-DAD). Other drugs of abuse were either detected via liquid chromatography with tandem mass spectromety (LC-MS/MS) and/or gas chromatography with (tandem) mass spectrometry (GC-MS(/MS))., Results: Ketamine plasma concentrations in a range of approx. 100-1200 ng/mL (mean: 510 ng/mL, median: 370 ng/mL) were detected. Co-consumption of at least one substance was ascertained in all cases. Besides driving impairments, recorded psychomotor impairments of the drivers comprised e.g. dilated pupils, missing or delayed pupil reactions, a slurred or decelerated speech, delayed reaction, lack of concentration, vertigo or agitation., Discussion: The observed peculiarities were in-line with literature data. However, the assessment and differentiation of ketamine-induced impairments was aggravated due to co-consumption of other drugs of abuse or pharmaceuticals in the herein investigated cases. Nevertheless, in two cases impairments can be attributed mainly to ketamine consumption since the co-consumed substances were only detected in low concentrations., Conclusion: The presented cases provide additional data on psychomotor impairments observed in ketamine-related DUID cases. Limiting factors are co-consumption of substances, unknown habituation to drugs and the limited case number. Nevertheless, the results of this study are comparable with existing literature data. Since the abuse of ketamine has increased in the past years, these data will support forensic casework., Competing Interests: Declaration of Competing Interest The authors have no relevant non-financial or financial conflicts of interest to disclose., (Copyright © 2023 Elsevier B.V. All rights reserved.)

Since 2020, our lab has received blood samples from traffic cases involving suspicion of driving under the influence of nitrous oxide (N 2 O). While N 2 O analysis by gas chromatography (GC) has been around for decades, quantitative results in blood from drivers have been only scarcely reported. We present a three-year (2020-2022) retrospective study of N 2 O from traffic cases in Eastern Denmark with suspected involvement of N 2 O intake. Whole blood samples from traffic cases were analysed for N 2 O using headspace-GC-MS. Freshly made calibration curves and additions of xenon gas as an internal standard were used for calculation of N 2 O concentrations. Positive samples have been defined as having concentrations greater than 0.1 mL N 2 O/L blood. Over a three-year period, we have tested 62 traffic case blood samples for the presence of N 2 O. Despite the technical challenges associated with the analysis of N 2 O, we have found N 2 O in 52 of the samples. Calculated concentrations were in the range 0.1-48 mL N 2 O/L blood, which are similar to the few cases previously found in the literature., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 The Authors. Published by Elsevier B.V. All rights reserved.)

Nyaope is a mixture of low grade heroin, cannabis products, antiretroviral drugs and other materials added as bulking agents. It is a highly physically additive mixture which is smoked by users. As part of the development of a method for the analysis and profiling of nyaope this study evaluates the stability of the cannabinoid, opiate and antiretroviral components of nyaope during storage following seizure. Conditions used were those typically used for storage of drug seizures: in a desiccator in a refrigerator, in a desiccator in the dark at room temperature, in a desiccator in daylight at room temperature and ambient room temperature in the dark in a cabinet used for storage of drug seizures. Street samples of cannabis (Δ9-tetrahydrocannabinol) and heroin were mixed with efavirenz and nevirapine tablets to mimic a nyaope sample. The samples were homogenized and transferred into glass bottles and extracted with tertiary butyl alcohol (tBuOH) and analysed by gas chromatography - mass spectrometry (GC-MS) after the powdered drugs had been stored for intervals of 0 and 24 h under each storage condition. The data obtained indicates that the target drug components in nyaope samples decompose and that for comparison purposes the drug extracts should be prepared in tBuOH immediately after seizure because of the decomposition of the drug components during storage prior to extraction and analysis. The implications of this work are that law enforcement agencies dealing with nyaope and wanting to compare drug samples may need to change their practice around how the drug is handled after seizure but prior to analysis. [ABSTRACT FROM AUTHOR]

A method based on gas chromatography-mass spectrometry (GC-MS) is described for the determination of venlafaxine, amitriptyline and duloxetine in human bone. Pulverized samples were incubated in methanol for 1 h under ultrasonication, after the addition of sertraline as internal standard. The samples were centrifuged, and the supernatants were evaporated. Samples were then resuspended in 0.1 M phosphate buffer pH 6 and subjected to solid phase extraction. Chromatography was performed on a fused silica capillary column and analytes were determined in the selected-ion-monitoring (SIM) mode. The assay was validated in the range 0.3-1 ng/mg (depending on the drug) to 500 ng/mg. The mean absolute recoveries ranged from 92.6% to 96.2%, the matrix effect from 76.9% to 103.3% and process efficiency from 74% to 95.9% depending on the analyte. The intra- and inter-assay accuracy values were always better than 20%. The validated method was then successfully applied to real bone samples from forensic cases in which toxicological analysis for these drugs in blood had been positive. Drugs were detected in bone in all blood positive results, the approximate concentrations being 36.4 ng/mg for amitriptyline, 19.3-3 ng/mg for duloxetine and 4.6-2 ng/mg for venlafaxine. [ABSTRACT FROM AUTHOR]

Cocaine was the second most widely used drug in Europe in 2016, with 3.5 million consumers aged 15-64 years old. Adulterants are pharmacologically active substances developed for medical purposes, however, there is little knowledge about their influence in the human body when there is concomitant use with cocaine. The objective of this work was to validate a method that allows the identification, confirmation and quantification of cocaine adulterants in blood samples collected in vivo or post-mortem. The studied substances were atropine, phenacetin, hydroxyzine, ketamine, lidocaine and tetramisole. A retrospective study of the prevalence of these substances, as well as their relative concentrations, was made analysing 97 real blood samples previously tested positive for cocaine and/or its metabolites. The analytes of interest were extracted, using a simple method based on protein precipitation with frozen acetonitrile and further analysis by GC/MS. The method was fully validated in accordance with parameters and criteria implemented in the lab and SWGTOX recommendations (mean recovery: 94-115%; CV: 6.2-13%; BIAS: 2.7-7.8%). 31 samples were positive for adulterants: phenacetin (19%), tetramisole (15%), lidocaine (8%) and hydroxyzine (1%). Concentrations were higher in post-mortem samples for all compounds analysed. Lidocaine was more prevalent in samples collected in vivo whereas tetramisole was present almost exclusively in post-mortem samples. Phenacetin was evenly distributed between post-mortem and in vivo samples. The validated method allows rapid, precise, accurate and economic analysis of selected compounds and requires smaller sample aliquots which can be important in post-mortem cases. The information collected can be important in future studies of correlation between the presence of adulterants and cocaine toxicity. [ABSTRACT FROM AUTHOR]

Triacetone triperoxide (TATP) is a high-power explosive which is often used by criminals. The detection of TATP is of great significance for solving the explosion cases. However, the preconcentration and analysis of trace levels of TATP still pose challenges for analytical researchers. In this study, metal-organic frameworks (MOFs), including IRMOF-8, MOF-5, UIO-66, ZIF-8, and MIL-101(Cr), were immobilized on a stainless steel wire using a physical adhesive method as a solid-phase microextraction (SPME) fiber coating. The prepared fibers with a controllable thickness were used for the extraction of TATP followed by gas chromatography-mass spectrometry (GC-MS) analysis. Under the identical experimental conditions, the IRMOF-8-coated fiber exhibited higher extraction efficiency for TATP than the other fibers. The IRMOF-8-coated fiber was then characterized using scanning electron microscopy and thermogravimetric analysis. The results indicated that the IRMOF-8-coated fiber not only had good thermal and chemical stabilities but also afforded a high TATP extraction efficiency. Under the same extraction conditions, the extraction efficiency of the IRMOF-8-coated fiber was 2–8 times higher than those of commercial fibers. The limit of detection was 13 ng/mL, and linearity was observed in the range of 50–5000 ng/mL with a correlation coefficient greater than 0.998. The intraday repeatability (n = 6), interday repeatability (n = 3), and fiber-to-fiber reproducibility (n = 3), were 4.1 %, 4.8 %, and 8.0 %, respectively. The recoveries of TATP from the simulated tap water and soil samples were 87.32–90.57 % and 88.76–100.93 %, respectively, with relative standard deviations lower than 11.11 % (n = 3). The above method was successfully applied for the detection of TATP transferred from a finger to a paper surface, demonstrating its good application prospects in the analysis of trace TATP. • MOF-based SPME fibers were prepared to extract TATP. • The extraction efficiencies of different MOF-coated fibers were compared. • Good stabilities and extraction efficiencies were obtained for IRMOF-8-coated fiber. • Extraction efficiency of IRMOF-8-coated fiber was higher than for commercial fibers. [ABSTRACT FROM AUTHOR]

Background: Retrograde extrapolation of drug concentrations in blood can be relevant in cases of drug-impaired driving and is regularly used in forensic toxicology in Norway. Δ 9 -tetrahydrocannabinol (THC) has complex, multi-compartmental pharmacokinetics, which makes retrograde extrapolation of blood THC concentrations problematic. In the present study, we evaluated an approach to retrograde extrapolation in which momentary rates of decrease of THC were estimated from two consecutive blood samples in apprehended drivers., Material and Methods: Data were collected from apprehended drivers in Norway 2000-2020. We included 548 cases in which THC was detected in two consecutive blood samples collected ≥ 20 min apart. THC concentrations were measured by GC-MS and UHPLC-MS/MS. In each case, THC concentrations and the time between the two sampling points (Δt) were used to estimate the rate constant k. The relationship between THC concentration and k was modelled by linear regression., Results: The median Δt was 31 min (interquartile range, IQR = 9). The median blood THC concentration was 2.4 μg/L (IQR = 3.4) at the first sampling point and 2.3 μg/L (IQR =3.1) at the second. The concentration decreased in 62% and increased in 38% of all cases. However, considering measurement uncertainty, the changes were not statistically significant in 87% of cases. The mean of k was 0.12 h -1 , corresponding to an apparent t 1/2 of 6.0 h. The t 1/2 predicted from linear regression of k against THC concentration ranged from 0.93 to 13 h for the highest and lowest concentrations observed (36 and 0.63 μg/L, respectively). The time from driving to blood collection had a median of 1.7 h (IQR = 1.5), and did not correlate with k., Conclusions: The apparent t 1/2 of THC calculated from the mean of k was 6.0 h, which is shorter than the terminal elimination t 1/2 suggested in previous population studies. This indicates that blood samples were often taken during the late distribution phase of THC. Because Δt was short relative to the rates of decrease expected in the late distribution and elimination phases, the underlying true concentration changes related to in vivo pharmacokinetics were small and masked by the relatively larger "false" changes introduced by random analytical and pre-analytical error. Therefore, individual values of k calculated from only two blood samples taken a short time apart are unreliable, and a two-sample approach to retrograde extrapolation of THC cannot be recommended., Competing Interests: Declaration of Competing Interest The authors declare the following financial interests/personal relationships which may be considered as potential competing interests: Gudrun Høiseth acts as an expert witness for Norwegian courts in cases and issues regarding forensic toxicology. Liliana Bachs acts as an expert witness for Norwegian courts in cases and issues regarding forensic toxicology. Cecilie H. Thaulow acts as an expert witness for Norwegian courts in cases and issues regarding forensic toxicology. Merete S. Vevelstad acts as an expert witness for Norwegian courts in cases and issues regarding forensic toxicology. Jørg Mørland is member of the Norwegian Board of Forensic Medicine and acts as an expert witness for Norwegian courts in cases and issues regarding forensic toxicology. Maren Cecilie Strand is member of the Norwegian Board of Forensic Medicine, Toxicological group, and acts as an expert witness for Norwegian courts in cases and issues regarding forensic toxicology. Peder Olai Skjeflo Holman has no conflicts of interests., (Copyright © 2023 The Authors. Published by Elsevier B.V. All rights reserved.)

Nyaope, a street drug commonly found in South Africa, is a mixture of low grade heroin, cannabis products, antiretroviral drugs and other materials added as cutting agents. It is a highly physiologically addictive substance which is smoked by users. Little work has been published on the chemical analysis and profiling of nyaope. Sample preparation prior to chromatographic or spectrometric analysis normally involves dissolution of the sample in an organic solvent. This study determined the most suitable organic solvent in which the common components of nyaope, namely Δ9-tetrahydrocannabinol, diamorphine, caffeine, dextromethorphan, phenacetin and the antiretrovirals efavirenz and nevirapine, which have different chemical characteristics, are stable during extraction and prior to analysis of nyaope samples i.e. autosampler stability. Street samples of cannabis (Δ9-tetrahydrocannabinol), heroin (diamorphine) and antiretrovirals were mixed to mimic a nyaope sample and dissolved in the organic solvents dichloromethane, ethanol, ethyl acetate, hexane, isopropanol and tertiary butyl alcohol. Analysis was performed after intervals of 0, 1, 6, 8, 24, 48 and 72h, prior to analysis by gas chromatography-mass spectrometry. Tertiary butyl alcohol resulted in the most stable extracts of the main nyaope components after 72h of storage. The analysis was also repeated on actual street samples of nyaope. These results show that tertiary butyl alcohol is a suitable solvent for sample preparation for the identification, comparison and profiling of nyaope samples. [ABSTRACT FROM AUTHOR]

Impurity profiling is a well described forensic tool that may be applied to gain information about the illegal drug market. However, it requires experience to assess the correlation between chemical profiles thereby separating linked from unlinked samples. One of the challenges in this context is that the chemical profiles may change over time, thus complicating an assessment if samples are stored under different conditions. In this study, the impact of different storage conditions on the stability of amphetamine impurity profiles was investigated. We examined the influence of storage time, temperature, sample purity, sample quantity and the presence of methanol on the amphetamine profile stability when stored for up to 12 months. We find that the target compounds in amphetamine impurity profiles are susceptible to all the examined storage conditions. Consequently, this unstable nature of amphetamine profiles may complicate the assessment when comparing amphetamine seizures that has been separated for longer time periods or stored under different conditions prior to seizure. Knowledge about the seizure history is rarely available to the forensic analyst. Therefore, sample stability issues should be taken into account when comparisons of chemical profiles are made. [ABSTRACT FROM AUTHOR]

For different reasons, street cocaine is often diluted with pharmacologically active substances, the so-called adulterants such as levamisole or hydroxyzine. A controversial debate exists currently on the uptake of adulterants from cocaine preparations and drug-related death. Previous research convincingly argues that serious adverse side effects that affect the central nervous and cardiovascular systems can be a consequence of adulterated cocaine.Aims: Having identified the presence of adulterants in lung tissue and blood, the concentrations of these substances in brain, an important target location, was of interest. This provides an opportunity to assess their role in cases of drug-related deaths.Materials and Methods: We developed and validated a method for the analysis of cocaine, two cocaine metabolites and six adulterants, which can typically be found in cocaine preparations, and one adulterant metabolite in brain tissue by gas chromatography-mass spectrometry (GC-MS)1. Ten brain samples which were tested positive for cocaine were analyzed. The homogenized brain tissue was embedded into drying paper for protein precipitation. During a subsequent solid-phase extraction (SPE), the eluate and one of the wash fractions were collected. After derivatization with N-Methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) in pyridine and isooctane, the extracts were analyzed by GC-MS.Results and Discussion: The method was fully validated for cocaine (COC), benzoylecgonine (BZE), ecgonine methyl ester (EME), diltiazem (DIL), hydroxyzine (HYD), and levamisole (LEV) and partly validated for cetirizine (CET), lidocaine (LID), phenacetin (PHE), and procaine (PRO) in brain material. By analyzing post-mortem brain tissue of ten cocaine users, LEV, LID, and HYD as well as PHE were identified in contrast to DIL, PRO, and the HYD metabolite CET. HYD and LEV were found in moderate to high concentrations in some cases. Therefore, it cannot be excluded that they have caused adverse side effects.Conclusion: Because adulterants can potentially affect the central nervous and cardiac systems, it is likely that they enhance COC toxicity. [ABSTRACT FROM AUTHOR]

Cocaine is usually trafficked from South America throughout the world in packages of approximately one kilogram shaped as bricks and imprinted with a logo. Seizures consisting of multiple cocaine bricks gives the opportunity to examine the variation in the chemical profile within cocaine bricks assumed to originate from the same manufacturer and maybe even the same production batch. This knowledge may be important to the forensic investigator when chemical profiles from cocaine samples of unknown origin are compared. In the present study, the alkaloid and residual solvent profiles from three large cocaine seizures each containing identical cocaine bricks was examined. The three cases consisted of 36, 84 and 100 cocaine bricks, respectively. Each cocaine brick was profiled according to its cocaine alkaloid and residual solvent content using gas chromatography-mass spectrometry (GC-MS) and headspace GC-MS. The study showed that each of the three identical looking seizures consisted of up to four groups of cocaine bricks displaying the same cocaine alkaloid and residual solvent profile. The size of the groups varied from 2.4 to 63.3kg cocaine. The study also showed that the residual solvent profile within each of the three large seizures exhibited very little variation whereas the alkaloid profile varied considerably more. This finding suggest that the same organic solvent is used for the production of several batches of cocaine HCl. Therefore, the residual solvent profile may be a tool to link different production batches from the same manufacturer even though the alkaloid profile are different. [ABSTRACT FROM AUTHOR]

A method for the statistical comparison of mass spectral data is demonstrated for applications in controlled substance analysis. The method uses an unequal variance t-test at each mass-to-charge ratio in the scan range to determine if two spectra are statistically associated or discriminated. If the two spectra are associated, a random-match probability is calculated to estimate the likelihood that the mass spectral fragmentation pattern in question occurs by random chance alone. If the two spectra are discriminated, the fragment ions responsible for the discrimination are determined. In this work, mass spectral data from case samples containing amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), phentermine, and psilocin were investigated. All spectra were collected in an accredited forensic laboratory using routine methods for controlled substance analysis. Using the statistical method, spectra of case samples were statistically associated to the corresponding reference standard at the 99.9% confidence level. In these instances, random-match probabilities ranged from 10-39 to 10-29, indicating the probability that the characteristic fragmentation pattern occurred by random chance is extremely small. Further, spectra of case samples were discriminated from other reference standards at the 99.9% or 99.0% confidence level, with 1-26 ions responsible for discrimination in each comparison. [ABSTRACT FROM AUTHOR]

The lipid composition of natural fingermarks was studied and compared with the composition of groomed residue. Approximately 100 specimens were collected from 6 donors over three sessions (in October, December and July) and analysed using gas chromatography / mass spectrometry (GC/MS). The measured lipid content was generally lower and more variable in natural fingermarks than in groomed fingermarks. Some significant variability was noticed. Relative standard deviations were the highest between donors (generally above 100%) but were also relatively high within donor within a session (from 21% to 80%) and between sessions (from 34% to 126%). The fingermarks from one of the donors generally contained higher relative amounts of lipids in both groomed and natural residue compared to the others. All other fingermarks led to very variable amounts and did not allow classifying the other donors as constantly "good" or "poor" donors. Squalene was the major compound in all marks, particularly in groomed specimens. A correlation between squalene, cholesterol, myristic acid, palmitoleic acid, stearyl palmitoleate and pentadecanoic acid was highlighted. Oleic and stearic were also correlated together but generally more in natural than groomed marks. The obtained results may be particularly useful to better understand the detection mechanisms for techniques targeting lipids and to develop artificial fingermark secretions to further support the development of detection techniques., (Copyright © 2023 The Authors. Published by Elsevier B.V. All rights reserved.)

Many different groups of chemical compounds can be used in statistical impurity-profile comparison in order to establish links between different seizures of illicit drugs. For cocaine, some of these compounds descent directly from the coca leaf while others are remnants from the manufacturing process; and each of the compound groups exhibit different degrees of stability and discrimination power. Information obtained from the different groups can be handled in numerous ways and selecting the right method using a balanced combination of the compound groups is highly important in order to provide investigators and courtrooms with accurate conclusions. By using logistic regression or discriminant analysis (linear and quadratic), cocaine alkaloid and residual solvent distances can be combined in order to obtain probabilities for the two possibilities: linked or unlinked. We examined different data transformations and distance methods and ranked the different models using cross validation. Validation in an unrelated data set proved the consistency of the results. Data consisted of five large groups of linked samples exposed to different storage conditions during 12 months, 124 different cocaine sample seizures and 15 smaller groups of linked samples stored at room temperature for up to 15 months. The alkaloid and residual solvent impurity profiles of the samples were analysed using gas chromatography-mass spectrometry (GC-MS) and headspace GC-MS, respectively. Residual solvent profiles exhibited considerable higher discrimination power than cocaine alkaloid profiles. Thus, a residual-solvent-weighted model (log10 transformation and cosine distance) was found superior at distinguishing correctly between linked and unlinked seizures compared to models using alkaloid distance alone. The model only gives weight to the residual solvents when the alkaloid profiles are very similar. This finding demonstrates the possibility to combine information from the highly stable, non-coca leaf-descent residual solvent profiles and the less stable cocaine alkaloid profiles for statistical comparative analysis of cocaine seizures in a simple and easy-to-implement way. [ABSTRACT FROM AUTHOR]

A method for identification and quantification of 2-methoxyqualone, an newly emerging quinazolinone derivative recreational drug, in human scalp hair was established using gas chromatography (GC)-tandem mass spectrometry (MS/MS). In this report, authentic cases are presented, in which the suspects were seized by police security bureau; the police in China requested our laboratory to identify and quantify the involved drug(s) of abuse in the hair samples of the suspects. After washing and cryo-grinding the authentic hair samples, the target compound was extracted with methanol, and the solvent layer was evaporated to dryness. The residue was reconstituted in methanol and analyzed by GC-MS/MS. 2-Methoxyqualone concentrations in the hair were between 35.1 and 116 pg/mg. The calibration curve of the substance in hair samples showed a good linearity in the concentration range of 10-1000 pg/mg (r > 0.998); the extraction recovery rate, 88.8-105.6 %; the interday and intraday precisions and accuracies (biases), not greater than 8.9 %. 2-Methoxyqualone in human hair had good stability under three different storage conditions at room (20 °C), refrigerated (4 °C) and frozen (- 20 °C) temperatures for at least 7 days. In the present report, simple and rapid quantification method for 2-methoxyqualone in human scalp hair have been established using GC-MS/MS and it could successfully be applied to authentic forensic toxicological cases. To our knowledge, this is the first report for quantification of 2-methoxyqualone in human hair samples., Competing Interests: Declaration of Competing Interest The authors declare the following financial interests/personal relationships which may be considered as potential competing interests: National Natural Science Foundation of China (Grant no. 81860331)., (Copyright © 2023. Published by Elsevier B.V.)

The actual illicit market for synthetic drugs is characterized by a wide variety of psychoactive substances of different chemical and pharmacological classes, such as amphetamine-type stimulants and new psychoactive substances. The knowledge about its chemical composition, as well as the nature and quantity of the active substances present, is important for emergency care in intoxication cases by these substances and to establish adequate chemical and toxicological analysis procedures in forensic laboratories. The aim of this work was to study the prevalence of amphetamine-type stimulants and new psychoactive substances in the states of Bahia and Sergipe, in the northeast region of Brazil, involving samples of drugs seized by the local police forces from 2014 to 2019. In a total of 121 seized and analyzed samples, in which ecstasy tablets predominated (n = 101), nineteen substances were identified using GC-MS and 1 D NMR techniques, comprising classical synthetic drugs and new psychoactive substances (NPS). In order to determine the composition of ecstasy tablets, an analytical method based on GC-MS was applied after validation. Analyzes of 101 ecstasy tablets showed that MDMA was the main substance, being found in 57% of the samples, in amounts between 27.3 and 187.1 mg per tablet. In addition, mixtures of MDMA, MDA, synthetic cathinones and caffeine were observed in 34 samples. These results demonstrate that the variety of substances found and the composition of seized materials in northeast Brazil is similar to other studies carried out previously in other Brazilian regions., Competing Interests: Conflict of interest The authors declare that they have no conflict of interest., (Copyright © 2023 Elsevier B.V. All rights reserved.)

This is a case report of a fatal intoxication in Cyprus related to 3,4-methylenedioxypyrovalerone (MDPV) and 2-(methylamino)-1-phenylpentan-1-one (pentedrone) intake combined with antipsychotic and antidepressant substances. A 42- year old man with a history of serious psychiatric illness was found unresponsive in his bed. Seized materials were also found close to his body. The forensic autopsy reported myocardial infarction due to multidrug intoxication. Toxicology screening in blood and urine was applied. Biological specimens were analysed by enzyme immunoassay procedure and GC/MS. MDPV, pentedrone and etizolam detected and quantitated in blood and urine. Other drugs quantitated in blood were also olanzapine, mirtazapine, and ephedrine. This was the first fatal case reported in Cyprus associated with new psychoactive substances. Additionally, this was the first case reported to Early Warning System of the European Monitoring Center of Drugs and Drug Abuse (EMCDDA), related to multidrug intoxication, attributed to the consumption of cathinones, designer benzodiazepines, and other drugs. [ABSTRACT FROM AUTHOR]

During the lifetime of a cocaine batch from production end to consumption, several alterations may occur, leading to possible changes in the original impurity profile. Such profile changes may eventually result in erroneous forensic evaluations. In the present study, the stability of both the alkaloid and the residual solvent impurity profiles of cocaine were evaluated over a period of 12 months under different storage conditions (temperature, purity and weight) using GC-MS and HS-GC-MS, respectively. The sample purity (p<0.001), time of storage (p<0.001) and storage temperature at 37°C (p<0.01) significantly influenced the alkaloid impurity profile. The most significant change was observed in low purity samples stored at 37°C. In contrast, no changes were observed in the residual solvent profile at all storage conditions for the entire 12-month study period. This finding indicates that the residual solvent profile may be more applicable than the corresponding alkaloid profile when cocaine seizures subjected to different storage conditions are compared. Our results clearly demonstrate that cocaine alkaloid profiles change over time and are most susceptible to sample purity and storage temperature. As a consequence, storage conditions and purity should be taken into account when cocaine comparison is conducted in criminal cases. [ABSTRACT FROM AUTHOR]

The ability to determine the post-mortem interval (PMI) in complex death investigations involving human remains, is a vital task faced by law enforcement. Establishing the PMI in a case can significantly aid in the reconstruction of forensically relevant events surrounding that death. However, due to the complexities surrounding the decomposition of human remains, the determination of the PMI still remains a challenge in some cases. Thus, the identification of biomarkers of human decomposition are an emerging, and essential, area of research. Previous studies have also demonstrated great success in the use of textiles as a host to indirectly capture decomposition by-products. This study reports the successful adaptation and optimisation of an analytical chemical workflow for the targeted analysis of lipids from textiles associated with decomposing human remains using gas-chromatography (GC) coupled with tandem mass spectrometry (MS/MS). This study discusses novel information regarding the complex challenges of matrix effects observed with decomposition samples. In addition, the first lipid profiles obtained from textiles associated with two decomposing human donors from the Australian Facility for Taphonomic Experimental Research (AFTER) using GC-MS/MS are presented., Competing Interests: Conflict of Interest The authors declare that there is no conflict of interest., (Copyright © 2023 Elsevier B.V. All rights reserved.)