Illicit Drug Samples Research Articles

Structure-Activity Relationships of the Fentanyl Scaffold: Identification of Antagonists as Potential Opioid Overdose Reversal Agents.

Opioid-related overdoses account for almost half of all drug overdose deaths in the United States and cause more preventable deaths every year than car crashes. Fentanyl, a highly potent mu opioid receptor (MOR) agonist and its analogues (fentalogues) are increasingly found in illicit drug samples, both where the primary drug of abuse is an opioid and where it is not. The prevalence of fentalogues in the illicit drug market is thought to be the primary driver of the increased number of opioid-related overdose deaths since 2016. In fact, fentanyl and its analogues are involved in more than 70% of opioid-related overdoses. The standard opioid overdose rescue therapy naloxone is often insufficient to reverse opioid overdoses caused by fentalogue agonists under current treatment paradigms. However, the pharmacology of many fentalogues is unknown. Moreover, within the fentalogue series of compounds, it is possible that antagonists could be identified that might be superior to naloxone as opioid overdose reversal agents. In this report, we explore the pharmacology of 70 fentalogues and identify compounds that behave as MOR antagonists in vitro and demonstrate with one of these reversals of fentanyl-induced respiratory depression in the mouse. Such compounds could provide leads for the development of effective agents for the reversal of opioid overdose.

Profiling of seized Cannabis sativa L. flowering tops by means of microwave-assisted hydro distillation and gas chromatography analyses

This research aimed to support police forces in their battle against illicit drug trafficking by means of a multi-technique approach, based on gas chromatography. In detail, this study was focused on the profiling of volatile substances in narcotic Cannabis sativa L. flowering tops. For this purpose, the Scientific Investigation Department, RIS Carabinieri of Messina, provided 25 seized samples of Cannabis sativa L. The content of Δ9-tetrahydrocannabinol (THC), useful to classify cannabis plant as hemp (≤ 0.2 %) or as marijuana (> 0.2 %), was investigated. Essential oils of illicit drug samples were extracted using a microwave-assisted hydro-distillation (MAHD) system; GC–MS and GC-FID analytical techniques were used for the characterization of the terpenes and terpenoids fingerprint. Furthermore, the enantiomeric and carbon isotopic ratios of selected chiral compounds were investigated using a heart-cutting multidimensional GC (MDGC) approach. The latter exploited a combination of an apolar column in the first dimension, and a chiral cyclodextrin-based column in the second one, prior to parallel isotope-ratio mass spectrometry (C-IRMS) and MS detection. Finally, all the data were gathered into a statistical model, to demonstrate the existence of useful parameters to be used for the classification of seized samples.

3D-printed portable device for illicit drug identification based on smartphone-imaging and artificial neural networks

In this manuscript, a 3D-printed analytical device has been successfully developed to classify illicit drugs using smartphone-based colorimetry. Representative compounds of different families, including cocaine, 3,4-methylenedioxy-methamphetamine (MDMA), amphetamine and cathinone derivatives, pyrrolidine cathinones, and 3,4-methylenedioxy cathinones, have been analyzed and classified after appropriate reaction with Marquis, gallic acid, sulfuric acid, Simon and Scott reagents. A picture of the colored products was acquired using a smartphone, and the corrected RGB values were used as input data in the chemometric treatment. ANN using two active layers of nodes (6 nodes in layer 1 and 2 nodes in layer 2) with a sigmoidal transfer function and a minimum strict threshold of 0.50 identified illicit drug samples with a sensitivity higher than 83.4 % and a specificity of 100 % with limits of detection in the microgram range. The 3D printed device can operate connected to a rechargeable lithium-ion cell portable battery, is inexpensive, and requires minimal training. The analytical device has been able to discriminate the analyzed psychoactive substances from cutting and mixing agents, being a useful tool for law enforcement agents to use as a screening method.

Recovery of DNA from acetaminophen exploring physical state and sampling methods

Research into the recovery of DNA from illicit drug samples has shown it is possible to get forensically useful profiles from such substrates. However, it is not yet known if the different physical states that drugs can be found in influences the quantity and quality of DNA that can be recovered or what is the best sampling method to adopt for powdered samples. This research used acetaminophen in four different states – large crystalline, powder, in solution, or residue – to determine the efficacy of current DNA technology in recovery and analysis of the resulting sample. Five replicates of each were prepared. Human blood was deposited on or mixed with the drug and left for 1 hour. The surface of the drug was sampled by wet/dry swabbing (where appropriate), or the entire sample was deposited in a tube, and the DNA then extracted using DNA-IQ™. The amount of DNA recovered (ng), degradation index, number of PCR cycles (Ct) required for the IPC to reach threshold, number of alleles in the DNA profile and average peak height (APH) were assessed. All samples, irrespective of the physical state they were collected from, returned full DNA profiles that corresponded to the DNA profile of the blood donor, with no degradation or inhibition detected. It was also found the wet/dry swabbing method returned higher levels of DNA than inclusion of the entire sample into the tube for powdered acetaminophen and the appropriate method to use will be dependent on casework circumstances. The findings of this research further develops our understanding of the recovery of DNA from drugs, and supports the need for further investigation to understand under what conditions DNA can be recovered from illicit substances.

Adulterants present in the San Diego county fentanyl supply: a laboratory analysis of seized law enforcement samples

BackgroundThe opioid overdose crisis is one of the worst public health crises ever to face the US and emerging evidence suggests its effects are compounded by the presence of drug adulterants. Here we report our efforts to characterize the adulterants present within the local fentanyl supply of San Diego County, obtained from undifferentiated drug samples seized by local law enforcement over the calendar year 2021.MethodsThirty-two participating local law enforcement agencies across San Diego submitted 4838 unknown individual illicit drug samples (total of 312 kg) to the San Diego County Sheriff’s Department Regional Crime Laboratory for identification.ResultsQualitative analysis of these samples via FTIR and GC-MS identified methamphetamine (38.7%), fentanyl (20.8%), diacetylmorphine (heroin) (10.2%), codeine (5.8%) and alprazolam (4.3%) as the most common illicit substances and the presence of 52 unique adulterants. The most common adulterants included 4-methylaminoantipyrine (4-MAAP) (10.9%), mannitol (9%), acetaminophen (8.5%), methamphetamine (4.2%), diacetylmorphine (heroin) (3.6%), tramadol (1.9%), and xylazine (1.7%). Several additional pharmacologically active adulterants and contaminants of interest were also identified.ConclusionThis analysis is vital for public health use and harm reduction efforts at the level of the individual consumer. Continued direct surveillance of the drug supply is necessary for the detection of potentially harmful adulterants that may pose serious threats to the public.

A survey of North American drug checking services operating in 2022

BackgroundDrug overdose deaths have reached record-breaking levels in North America. Drug checking services (DCS) provide localized information on the contents of drugs to individuals and communities. Depending on the design, individuals can submit drug samples for onsite “real-time” testing or offsite testing. The results can shed light on emerging drugs in the community and support ongoing prevention and surveillance efforts. We sought to describe and report aggregate outcomes of DCS operating in North America. MethodsThe North American Drug Checking Survey was launched in 2022 to characterize and monitor DCS operating in the region. Sixteen organizations from the US (n = 9), Canada (n = 5), and Mexico (n = 2) responded to the survey. Each organization reported on their program's operations and provided service delivery outcomes (site- or program-level) in the aggregate. ResultsParticipating organizations reported testing a total of 49,786 drug samples between 2014 and 2022. DCS were run by community-led organizations (44%), health departments (25%), universities (19%), or clinical/private laboratories (19%). The types of samples tested differed between programs (e.g., solids vs. liquids, drug paraphernalia accepted). While most organizations tested onsite using fentanyl test strips (88%) and Fourier-transform infrared (FTIR) spectroscopy (63%), many sent samples offsite for confirmatory testing (63%), most often with mass spectrometry. Common facilitators of operating a DCS included: interest of clients (69%), interest of service providers (63%), and receiving external technical assistance (63%). Barriers included: the lack of funding (81%) or staff (50%), gaps in technical expertise (38%), as well as laws banning the possession and/or distribution of illicit drug samples, drug paraphernalia, or drug checking equipment (38%). ConclusionDCS are scaling up in North America. Given the evolving and localized nature of illicit drug supplies, supporting the establishment and operations of DCS could enhance the public's understanding of local drug supplies to reduce drug-related harms over time.

Development and validation of a liquid chromatography tandem mass spectrometry method for the analysis of 53 benzodiazepines in illicit drug samples

An LC-MS/MS method for the analysis of 53 benzodiazepines, including various designer benzodiazepines, was developed. The developed method was applied to a total of 79 illicit street drug samples collected in Chicago, IL. Of these samples, 68 (84%) had detectable amounts of at least one benzodiazepine. Further, of the 53 benzodiazepines included in the developed method just 14 were measured in samples. Clonazolam, a potent designer benzodiazepine and derivative of clonazepam, was the most frequently measured benzodiazepine in 63% of samples and was measured in the highest concentrations. Other benzodiazepines measured in more than 10% of samples included clonazepam, alprazolam, flualprazolam, and oxazepam. Mixtures of benzodiazepines were frequently measured in samples, with just 24% of samples containing just one benzodiazepine. To determine the response of benzodiazepines on a rapid, point-of-use drug checking tool, all 53 benzodiazepine standards were screened on a lateral flow immunoassay benzodiazepine test strip. Sixty eight percent of standards gave a positive BTS response at a concentration of 20 µg/mL, demonstrating BTS have response to a wide variety of benzodiazepines, including many designer benzodiazepines. A comparison of this data to previous data reported for the same samples demonstrated all samples containing a benzodiazepine also had an opioid present, with fentanyl being present in 94% of benzodiazepine samples. These results highlight high rates of polysubstance drug presence in Chicago, IL illicit drug samples, posing an increased risk of drug overdoses in people who use drugs.

Validated method for the analysis of 22 illicit drugs and their metabolites via liquid chromatography tandem mass spectrometry (LC-MS/MS) in illicit drug samples collected in Chicago, IL.

Drug checking services are being utilized worldwide to provide people who use drugs information on the composition and contents of their drugs as a tool for harm reduction and accidental overdose prevention. Existing drug checking services use a variety of techniques including immunoassay strips and spectroscopic techniques like FTIR and Raman. Few services utilize LC-MS based methods for primary or secondary analysis and few methods exist for direct analysis of illicit drugs. To address this, an LC-MS/MS method was developed for 22 illicit drugs and cutting agents using LC-MS/MS with application to 124 illicit drug samples that were collected from Chicago, IL. Samples were also analyzed using fentanyl and benzodiazepine immunoassay test strips. Fentanyl test strips gave a positive result for 86% of samples with only one sample showing a positive result on a benzodiazepine test strip. LC-MS/MS analysis of samples show that opioids were the most commonly quantified in 96% of samples, followed by stimulants at 12% and benzodiazepines at 1%. Fentanyl was measured in 91% of samples, co-occurring with heroin in 58% of opioid-containing samples. A comparison of the gold-standard LC-MS/MS results to fentanyl test strips shows a high level of accuracy for the fentanyl test strips, with just 5% of samples being classified as false negatives and no false positives. These results demonstrate the strengths and benefits of LC-MS/MS when incorporated as a secondary analysis tool for drug checking.

Validated portable device for the qualitative and quantitative electrochemical detection of MDMA ready for on-site use

Identifying and quantifying 3,4-methyl​enedioxy​methamphetamine (MDMA) on-site in suspected illicit drug samples, whether it be at recreational settings or manufacturing sites, is a major challenge for law enforcement agencies (LEAs). Various analytical techniques exist to fulfil this goal, e.g. colourimetry and portable spectroscopic techniques, each having its specific limitations (e.g. low accuracy, fluorescence, no quantification) and strengths (e.g. fast, easy to use). In this work, for the first time, an electrochemical MDMA sensor is presented to become a detection tool that can realistically be used on-site. More specifically, the use of a single buffer solution and an unmodified screen-printed electrode, along with the integration of a data analysis algorithm and mobile application permits the straightforward on-site identification and quantification of MDMA in suspicious samples. Multiple studies investigating different parameters, including pH, concentration, reproducibility, temperature and binary mixture analyses, were executed. To fully understand all the occurring redox processes, liquid chromatography coupled with high-resolution mass spectrometry analysis of partially electrolyzed MDMA samples was performed unravelling oxidation of the methylenedioxy group. Validation of the methodology was executed on 15 MDMA street samples analysed by gas chromatography coupled with mass spectrometry and compared with the performance of a commercial portable Raman and Attenuated Total Reflection Fourier Transform Infrared Spectroscopy (ATR-FTIR) device. The novel methodology outperformed the spectroscopic techniques, correctly identifying all 15 street samples. Additionally, the electrochemical sensor predicted the purity of the tablets with a mean absolute error of 2.3%. Overall, this new, electrochemical detection strategy provides LEAs the rapid, low-cost, on-site detection and quantification of MDMA in suspicious samples, without requiring specialized training.

Development of qualitative GC MS method for simultaneous identification of PM-CCM a modified illicit drugs preparation and its modern-day application in drug-facilitated crimes

Prescriptions for psychoactive substances such as Pregabalin, Methamphetamine, Caffeine, Clonazepam and Mirtazapine (PM-CCM) are common in the treatment of a variety of disorders. Indeed, the PM-CCM has been used in different therapeutic areas, including insomnia, anxiety, seizure disorders, etc. Unfortunately, these psychoactive substances are present in the illegal street market, leading to a lot of drug abuse among some addicted users, road insecurity and suicide. Hence, it has become essential to validate and develop a rapid and effective method to analyze the PM-CCM, a modified illicit drug, for drug abuse in the forensic sciences. A simple, rapid, specific and sensitive Gas Chromatography-Mass Spectrometry(GC-MS) method has been developed for the identification of Pregabalin, Methamphetamine, Caffeine, Clonazepam and Mirtazapine (PM-CCM) in forensic exhibits. At room temperature, the sample was ultrasonicated for 5 minutes before being extracted with methanol. A highly precise auto-injector is used to inject a very small quantity of samples for analysis. Helium is used as a carrier gas with a flow rate of 1 ml/min. The separation of PM-CCM was performed on SH-RXi-5 MS, ID.25 mm, film thickness. 25 µm, length of 30 m column. The constituents of PM-CCM were identified by the mass-to-charge ratio (m/z ratio) of fragments of the parent compound by comparing them with the NIST-17 MS Library. Separation and identification of PM-CCM were achieved within a 15-minute run. The proposed method has been successfully used for the routine analysis of PM-CCM in complex illicit drug preparations and in forensic exhibits as well. The application of above discussed qualitative analysis method and screening of PM-CCM, modified illicit drug samples demonstrates the potential and applicability of the technique to the fast chemical profiling of illicit samples.

Progress on the Electrochemical Sensing of Illicit Drugs.

Illicit drugs are harmful substances, threatening both health and safety of societies in all corners of the world. Several policies have been developed over time to deal with this illicit drug problem, including supply reduction and harm reduction policies. Both policies require on-site detection tools to succeed, i.e. sensors that can identify illicit drugs in samples at the point-of-care. Electrochemical sensors are highly suited for this task, due to their short analysis times, low cost, high accuracy, portability and orthogonality with current technologies. In this chapter, we evaluate the latest trend in electrochemical sensing of illicit drugs, with a focus on detection of illicit drugs in seizures and body fluids. Furthermore, we will also provide an outlook on the potential of electrochemistry in wearable sensors for this purpose.

ANALYSIS AND SEPARATION OF COMMON ADULTERANTS AND DILUENTS FROM THE ILLICIT DRUG (HEROIN)SAMPLES

The drug trafficking problem in Rajasthan is quite common as Rajasthan is the largest state in India, and many international and interstate borders surround it. Illicit traffickers can add unlimited diluents and adulterants to heroin. Only 5% or less than that alkaloid is present; the rest is of diluents and adulterants. Adulterants can associate with a significant risk of overdose, which may lead to death due to severe poisoning. Thus, the purity of drugs may vary, and the presence and percentage of diluents and adulterants depend on the region. The present article aims to identify and separate diluents and adulterants from diacetylmorphine drug samples. The illicit drug samples were deposited for investigations in the narcotics division of the state forensic science laboratory, Jaipur. During studies, sophisticated instruments like GCMS confirmed the preliminary results obtained from TLC and color tests. The variety and quantity of adulterants and diluents differ in all the samples, but the pattern is similar. The extensive and widespread cutting agent of illicit drugs used to analyze these drug samples.

Evaluation and improvement of a miniature mass spectrometry system for quantitative harm reduction drug checking

The increasing variability of the illicit drug market has imposed serious health risks for people who use drugs (PWUD), particularly due to the increasing co-occurrence of opioids and etizolam (or other benzodiazepines) in some jurisdictions. A miniature mass spectrometer (MS) equipped with paper capillary spray ionization was evaluated for its ability to quantify fentanyl, fluorofentanyl, carfentanil, and etizolam in illicit drug samples. Prior to testing actual drug samples, inter- and intra-day reproducibility, calibration linearity, and analytical sensitivity were assessed. The development of a continuous spray solvent delivery system improved MS/MS quantitation by prolonging ionization stability. A simple, rapid and quantitative tandem mass spectrometry method was developed and employed for the analysis of real-world illicit drug samples provided by PWUD at a harm reduction site in Victoria, British Columbia, Canada. Limits of detection ranged from 0.001 to 0.24% w/w of illicit analyte in the original solid drug samples. Target analytes were detected and quantified via the miniature MS system for samples where conventional on-site drug checking technologies were not always effective. These promising results demonstrate the potential role for miniature mass spectrometer systems for on-site drug checking services that can be both sensitive to trace, toxic levels as well as adaptable/selective for new drug threats as they appear in the illicit drug supply.

Ionic liquids as stationary phases for the gas chromatographic separation of fentanyl analogues

The continuous emergence of novel fentanyl analogues has created a need for improved methods able to distinguish between fentanyl analogues and their isomers. In this study, the utility of commercially available ionic liquid columns is demonstrated for GC-FID and GC–MS separation and unambiguous identification of fentanyl, 22 fentanyl analogues and U-47700. The selectivity of the IL column towards these compounds was determined as well as the effectiveness of detection from complex illicitly synthesized drug samples. The results of this study were compared to a 5% diphenyl/95% dimethylpolysiloxane column to show increased selectivity and applicability towards seized illicit drug samples. 24 compounds were separated 36% faster with an elution window increase of 33% on the ionic liquid phase compared to the 5% diphenyl/95% dimethylpolysiloxane phase. The selectivity of 11 isomeric analogue sets (out of 12) increased by 2 to 25% over the 5% diphenyl/95% dimethylpolysiloxane phase showing an ionic liquid column is more favorable for separating fentanyl analogues. The ionic liquid column provides better signal to noise, and a faster and more selective option for forensic laboratories looking to identify confiscated illicit drug samples.

Development of a Graphene-Oxide-Deposited Carbon Electrode for the Rapid and Low-Level Detection of Fentanyl and Derivatives.

The opioid overdose crisis in North America worsened during the COVID-19 pandemic, with multiple jurisdictions reporting more deaths per day due to the fentanyl-contaminated drug supply than COVID-19. The rapid quantitative detection of fentanyl in the illicit opioid drug supply or in bodily fluids at biologically relevant concentrations (i.e., <80 nM) remains a significant challenge. Electroanalytical techniques are inexpensive and can be used to rapidly detect fentanyl, but detection limits need to be improved. Herein, we detail the development of an electrochemical-based fentanyl analytical detection strategy that used a glassy carbon electrode modified with electrochemically reduced graphene oxide (ERGO) via electrophoretic deposition. The resulting surface was further electrochemically reduced in the presence of fentanyl to enhance the sensitivity. Multiple ERGO thicknesses were prepared in order to prove the versatility and ability to fine-tune the layer to the desired response. Fentanyl was detected at <10 ppb (<30 nM) with a limit of detection of 2 ppb and a calibration curve that covered 4 orders of concentration (from 1 ppb to 10 ppm). This method was sensitive to fentanyl analogues such as carfentanil. Interference from the presence of 100-fold excess of other opioids (heroin, cocaine) or substances typically found in illicit drug samples (e.g. caffeine and sucrose) was not significant.

The versatility of the XRPD for the drug detection

The increasing prevalence of New Psychoactive Substances (NPS) on the drug market exerts considerable pressure on the development of novel detection techniques, especially those suitable for analyses directly on a crime scene. Raman and IR spectroscopy usually fulfil such needs; however, they have limitations (e.g. fluorescence in Raman and sometimes both Raman and IR have difficulties with identifying compounds in certain mixtures). For this reasons, we investigated the potential of X-ray powder diffraction (XRPD) for the identification of drug samples. Beyond identifying the actual controlled substances, this technique might also be very useful in identification of either organic or inorganic cutting agents. The sample crystals were crushed and flattened on the silicon pod to create a planar surface. Bruker D2 Phaser powder diffractometer with parafocusing Bragg–Brentano geometry using CuKα radiation (λ=1.5418 Å) was used for the measurement. The data were collected by an ultrafast LYNXEYE XE detector and subsequently evaluated using HighScore Plus 3.0e software. First, a series of 8 NPS standards was used to verify whether XRPD can distinguish between substances with similar chemical structures. The obtained XRPD patterns confirmed this ability. Subsequently, to verify the ability of XRPD to identify substances in real samples, a series of seized samples provided by Czech police was analysed by XRPD. The comparison of the obtained diffraction data with the patterns of the respective standards enabled their identification. Moreover, results from the analyses of cocaine street samples showed that XRPD might be able to detect not only the cocaine itself, but also the present cutting agents in a single run analysis. With respect to the physical basis of how the XRPD works, in case of mixtures, some signals in the diffraction pattern may overlap. However, if the overlap is only partial, identification of compounds in the unknown sample might still be possible with a proper database. XRPD was able to distinguish all the NPS despite their similar molecular structures and to identify each of the seized substances. Furthermore, XRPD was able to identify the main cutting agent in several samples of seized cocaine. These results show that XRPD could be a valuable analytical tool for the detection of both the unknown compounds and cutting agents in illicit drug samples.

Nanomaterial‐Based Sensor Arrays With Deep Learning for Screening of Illicit Drugs

AbstractRapid and accurate screening techniques are demanded for illicit drugs that have raised international tensions. Bovine serum albumin‐stabilized gold nanoclusters (BSA‐Au NCs), carbon dots (C dots), thiosalicylic acid‐stabilized silver nanoclusters (TA‐Ag NCs), and Marquis reagent as photoluminescent sensing probes for five common illicit drugs are demonstrated in this study. Cocaine, 4‐chloroethcathinone (4‐CEC), and ketamine induce different degrees of photoluminescence changes of BSA‐Au NCs, C dots, and TA‐Ag NCs. Detection of heroin and methamphetamine (MA) is based on their formation of fluorescence polymer particles with Marquis reagent. To provide a unique pattern for each analyte, 2 × 4 sensor arrays are prepared. A deep learning‐drug screening platform and system (DL‐DSPS) is established and applied to differentiate the five illicit drugs, each with unique code based on its response to the probes. For example, codes of (−1, −1, 1, 0), (0, −1, 1, 0), (0, 0, 1, 0), (0, 0, 1, 1), and (0, 0, 0, 1) are for 4‐CEC, cocaine, ketamine, heroin, and MA, respectively. The cost‐effective and compact DL‐DSPS is validated for screening of real‐world illicit drug samples, with results in good agreement with that from GC‐MS, showing its potential for multi‐drug screening at crime scenes.

Automatic analytical approach for the determination of 12 illicit drugs and nicotine metabolites in wastewater using on-line SPE-UHPLC-MS/MS

In this study, we developed a novel on-line solid phase extraction (SPE)-ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS)-based analytical method for simultaneously quantifying 12 illicit drugs and metabolites (methamphetamine, amphetamine, morphine, codeine, 6-monoacetylmorphine, benzoylecgonine, 3,4-methylenedioxymethamphetamine, 3,4-methylenedioxyamphetamine, cocaine, ketamine, norketamine, and methcathinone) and cotinine (COT) in wastewater samples. The analysis was performed by loading 2 mL of the sample onto an Oasis hydrophilic-lipophilic balance cartridge and using a cleanup step (5% methanol) to eliminate interference with a total run time of 13 min. The isotope-labeled internal standard method was used to quantify the target substances and correct for unavoidable losses and matrix effects during the on-line SPE process. Typical analytical characteristics used for method validation were sensitivity, linearity, precision, repeatability, recovery, and matrix effects. The limit of detection (LOD) and limit of quantification (LOQ) of each target were set at 0.20 ng/L and 0.50 ng/L, respectively. The linearity was between 0.5 ng/L and 250 ng/L, except for that of COT. The intra- and inter-day precisions were <10.45% and 25.64%, respectively, and the relative recovery ranged from 83.74% to 162.26%. The method was used to analyze various wastewater samples from 33 cities in China, and the results were compared with the experimental results of identical samples analyzed using off-line SPE. The difference rate was between 19.91% and −20.44%, and the error range could be considered acceptable. These findings showed that on-line SPE is a suitable alternative to off-line SPE for the analysis of illicit drugs in samples.

Can X-Ray Powder Diffraction Be a Suitable Forensic Method for Illicit Drug Identification?

New psychoactive substances (NPSs) are associated with a significant number of intoxications. With the number of readily available forms of these drugs rising every year, there are even risks for the general public. Consequently, there is a high demand for methods sufficiently sensitive to detect NPSs in samples found at the crime scene. Infrared (IR) and Raman spectroscopies are commonly used for such detection, but they have limitations; for example, fluorescence in Raman can overlay the signal and when the sample is a mixture sometimes neither Raman nor IR is able to identify the compounds. Here, we investigate the potential of X-ray powder diffraction (XRPD) to analyse samples seized on the black market. A series of psychoactive substances (heroin, cocaine, mephedrone, ephylone, butylone, JWH-073, and naphyrone) was measured. Comparison of their diffraction patterns with those of the respective standards showed that XRPD was able to identify each of the substances. The same samples were analyzed using IR and Raman, which in both cases were not able to detect the compounds in all of the samples. These results suggest that XRPD could be a valuable addition to the range of forensic tools used to detect these compounds in illicit drug samples.

Identification and Confirmation of Fentanyls on Paper using Portable Surface Enhanced Raman Spectroscopy and Paper Spray Ionization Mass Spectrometry

Fentanyl and its analogues play a major role in the current opioid epidemic. In particular, these highly potent opioids have become a health hazard due to their use as additives in street drugs. Consequently, rapid on-site procedures for the analysis of this class of seized drugs are needed, especially considering the reported backlog of drug samples, which must undergo identification and confirmation tests to validate the presence of an illicit substance. Paper based devices are cheap sampling and analysis vehicles that have been shown capable of allowing rapid identification and confirmation of drugs of abuse. Modifying paper substrates by imprinting nanoparticles enables surface enhanced Raman spectroscopy (SERS) as well as a second analysis from the same substrate, namely paper spray ionization mass spectrometry. While such a procedure has been described for laboratory use, these illicit drug samples are typically collected in the field and this is where testing should be done. We combine paper SERS and paper spray MS on field-portable and commercial off-the-shelf (COTS) devices for the rapid and low-cost identification and confirmation of fentanyl and its analogues, enabling in situ analysis at the point of seizure of suspect samples. The commercial nature of both instruments moves this technology from the academic realm to a setting where the criminal justice system can realistically utilize it. The capabilities of this single-substrate dual-analyzer technique are further examined by sampling a variety of surfaces of forensic interest.