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Research suggests that hair color, hair dyeing, and perspiration can bias hair test results regarding drug exposure, but research is needed to examine such associations in a multivariable manner. In this epidemiology study, adults were surveyed entering nightclubs and dance festivals in New York City, and 328 provided hair samples, which were analyzed using ultra-high-performance liquid chromatography-tandem mass spectrometry to determine the level of detection of cocaine and 3,4-methylenedioxymethamphetamine (MDMA). Reporting use was not an inclusion criterion for analysis. We used two-part multivariable models to delineate associations of hair color, past-year hair dyeing, and frequency of past-month hat wearing (which may increase perspiration) in relation to any vs. no detection of cocaine and MDMA as well as level of detection, controlling for hair length, self-reported past-year cocaine/ecstasy/MDMA use, and age, sex, and race/ethnicity. Those reporting having dyed their hair were at increased odds of having any level of cocaine detected (adjusted odds ratio [aOR] = 3.75, 95% CI confidence interval [CI]: 1.85-6.70), and compared to those with brown hair, those with blond(e) hair on average had lower levels of cocaine (ng/mg) detected (beta = -7.97, p = 0.025). Those reporting having dyed their hair were at increased odds of having any level of MDMA detected (aOR = 3.05, 95% CI: 1.44-6.48), and compared to those who reported never wearing a hat, those who reported wearing a hat daily or almost daily on average had lower levels of MDMA (ng/mg) detected (beta = -6.61, p = 0.025). This study demonstrates the importance of using multivariable models to delineate predictors of drug detection., (© 2023 John Wiley & Sons, Ltd.)

Hair testing is a useful tool to investigate suspected pediatric exposure to drugs of abuse. Newborns and young children are at high risk of exposure to drugs of abuse from parents or caregivers who consumed these substances, a fact prosecuted by Spanish authorities as child abuse. A retrospective study based on a cohort of 37 cases classified using several parameters, which involve children under 12 years old, were analyzed at the Drugs Laboratory of the National Institute of Toxicology and Forensic Sciences (Madrid, Spain) between 2009 and 2021. Hair samples were tested for the presence of opiates, cocaine, ketamine, amphetamines, methadone, and cannabis using a gas chromatography-mass spectrometry (GC-MS) method. A 59% of the studied children had ages in the range of 1-3 years old, and in 81% of cases, victims required hospitalization. In 81% of cases (n = 30), hair was submitted only or in combination with other samples, and these were classified in four categories according to analyzed samples: A (only hair), B (hair and blood), C (hair and urine), and D (hair, blood, and urine). The 93.3% of these cases (n = 28) showed a positive result of cannabinoids (THC and CBN in hair and THC-COOH in urine; 71.4% n = 20), cocaine and metabolites (benzoylecgonine and cocaethylene; 46.4% n = 13), opiates (morphine and 6-acetylmorphine), and amphetamines (MDMA and MDMA; 3.10% n = 1). Hair analysis matched positive results in cases where urine screening test was carried out previously (n = 24) and in those cases where blood and/or urine were also submitted (35.6% n = 11). As a conclusion, hair analysis was confirmed as a useful tool to detect previous exposure to acute poisoning events in children., (© 2023 John Wiley & Sons Ltd.)

The work discusses the results of hair and urine testing performed in 51 cases of suspected in utero drug exposure handled at the University Hospital of Verona from 2016 to 2022. On the day of birth or the day after birth, urine from mother and newborn (UM and UN) and hair from mother (HM), newborn (HN) and father (HF), if possible, were collected. Urine underwent immunoassay and GC-MS analysis, whereas hair underwent LC-MS/MS and GC-MS/MS analysis. In 50 out of 51 cases, HM and/or HN were available. In 92% of them, hair testing resulted in a positive, often (>50% cases) for more than one class of substance. The most detected substances were cocaine, opiates, methadone and cannabinoids. Maternal segmental analysis showed a prevalent decreasing concentration trend during pregnancy in case of positivity for one class of substances, whereas, as expected, a neatly prevalent increasing trend in the case of positivity for more than one class of substances. In nine cases, HF was also available, resulting in all being positive, usually for the same classes of substances identified in HM, thus questioning parental responsibility. In 33 cases, urine samples from the mother or newborn were also collected. Of them, 27 cases (82%) tested positive, showing peri-partum drug consumption and then confirming the severity of the addiction. Hair testing showed to be a reliable diagnostic tool to investigate in utero drug exposure because of the possibility of obtaining a complete picture of maternal addictive behaviour and family background, thanks to segmental maternal hair analysis and father hair testing., (© 2023 The Authors. Drug Testing and Analysis published by John Wiley & Sons Ltd.)

When developing a procedure to identify external contamination of hair as opposed to drug that is in hair from ingestion, there are components of the process that must be considered in the final method. A method that does not achieve the objective may be missing one or more of these elements: choice of solvent, a drug-binding agent, ratio of solvent to hair, temperature, time, intactness of the hair, and establishing, for the chosen method, a criterion based on the drug contents of the wash and hair that indicates the hair may be contaminated., (© 2022 John Wiley & Sons, Ltd.)

A method using innovative sample preparation was developed for determination of cocaine on banknotes. Aqueous extraction of cocaine from banknotes was performed using a sonication-enhanced technique. Quantitation of cocaine was achieved using high performance liquid chromatography (HPLC) with UV detection at 230 nm, whereas identification was accomplished utilizing gas chromatography with mass spectrometry (GC-MS). Multiple calibration techniques, including the external calibration method (ECM), internal standard method (ISM), and standard addition method (SAM) were incorporated into the experimental design to simultaneously determine cocaine contents and assess matrix effects. Statistical paired t tests confirmed that matrix effects were not significant with the sample preparation employed. No damage to the features of the banknotes was observed from the extraction procedure. Extraction efficiency, spike recovery, and detection limit were also determined. The unique experimental design allowed for ECM, ISM, and SAM to concurrently determine the contents of cocaine on banknotes collected around Metro-Detroit. The concentration range of cocaine was from 1.58 to 14.7 μg per note, with an average of 6.96 μg per note. The method is simple and suitable for drug analysis and forensic science applications., (© 2022 The Authors. Drug Testing and Analysis published by John Wiley & Sons Ltd.)

Human oral fluid is well established as a matrix for drug screening, particularly in the workplace. The need to synthesise synthetic oral fluid (SOF) has been recognised in order to overcome human oral fluid's composition variability. We have used SOF spiked with six common drugs of abuse or their primary metabolites: morphine, amfetamine, benzoylecgonine, cocaine, diazepam, and (-)-Δ 9 -tetrahydrocannabinol (THC) in order to assess the suitability of this matrix for quality assurance purposes. For confirmation of a drug screening test, controls and spiked standards are normally required. All our analytes were detected by LC-MS/MS using a quick and easy "dilute and inject" sample preparation approach as opposed to relatively slower solid-phase extraction. The limit of detection (LOD) was 10 ng/ml for diazepam and THC and 5 ng/ml for morphine, amfetamine, benzoylecgonine and cocaine. Validation results showed good accuracy as well as inter- and intra-assay precision (CV [%] < 5). Our work highlighted the importance of adding Tween® 20 to the SOF and calibrants to reduce losses when handling THC. Furthermore, drug stability was tested at various temperatures (5°C, 20°C and 40°C), for a number of days or after freeze-thaw cycles. Recommendations regarding storage are provided, the spiked SOF being stable at 5°C for up to 1 week without significant drug concentration loss., (© 2022 The Authors. Drug Testing and Analysis published by John Wiley & Sons Ltd.)

Illicit drug profiling performed by forensic laboratories assists law enforcement agencies through providing information about chemical and/or physical characteristics of seized specimens. In this article, a model was developed for the comparison of seized cocaine based on retrospective analysis of data generated from ultrahigh performance liquid chromatography with time-of-flight mass spectrometry (UHPLC-TOF-MS) comprehensive drug screening. A nontargeted approach to discover target compounds was employed, which generated 53 potential markers using data from cocaine positive samples. Twelve marker compounds were selected for the development of the final profiling model. The selection included a mixture of commonly used cocaine profiling targets and other cocaine-related compounds. Combinations of pretreatments and comparison metrics were assessed using receiver operating characteristic curves to determine the combination with the best discrimination between linked and unlinked populations. Using data from 382 linked and 34,519 unlinked distances, a classification model was developed using a combination of the standardization and normalization transformations with Canberra distance, resulting in a linked cut-off with a 0.5% false positive rate. The present study demonstrates the applicability of retrospectively developing a cocaine profiling model using data generated from UHPLC-TOF-MS nontargeted drug screening without pre-existing information about cocaine impurities. The developed workflow was not specific to cocaine and thus could potentially be applied to any seized drug in which there are both sufficient data and impurities present., (© 2021 The Authors. Drug Testing and Analysis published by John Wiley & Sons Ltd.)

The use of illicit drugs across the world causes issues for users, healthcare workers and the public. Therefore, rapid and reliable onsite testing methods to detect these drugs are required. In this study, seven commercial surface-enhanced Raman spectroscopy (SERS) substrates A-G were compared for the analysis of cocaine. These substrates were compared using scanning electron microscopy to study the surface structure and Raman spectroscopy and to determine if there was any enhancement of the cocaine bands. Substrate B provided the best enhancement of known cocaine vibrational bands, allowing the detection down to concentrations of 1 ng/mL in standards and 10 ng/mL extracted from the oral fluid. The results showed that SERS is an ideal method for future rapid onsite analysis of illicit drugs in oral fluid. Commercial SERS substrates were compared for the analysis of cocaine. Substrate B provided the best result and was further tested with lower concentrations and extracts from the oral fluid. The application to oral fluid testing could prove useful for future onsite analysis., (© 2020 John Wiley & Sons, Ltd.)

Handheld Raman spectroscopy is an emerging technique for rapid on-site detection of drugs of abuse. Most devices are developed for on-scene operation with a user interface that only shows whether cocaine has been detected. Extensive validation studies are unavailable, and so are typically the insight in raw spectral data and the identification criteria. This work evaluates the performance of a commercial handheld Raman spectrometer for cocaine detection based on (i) its performance on 0-100 wt% binary cocaine mixtures, (ii) retrospective comparison of 3,168 case samples from 2015 to 2020 analyzed by both gas chromatography-mass spectrometry (GC-MS) and Raman, (iii) assessment of spectral selectivity, and (iv) comparison of the instrument's on-screen results with combined partial least square regression (PLS-R) and discriminant analysis (PLS-DA) models. The limit of detection was dependent on sample composition and varied between 10 wt% and 40 wt% cocaine. Because the average cocaine content in street samples is well above this limit, a 97.5% true positive rate was observed in case samples. No cocaine false positives were reported, although 12.5% of the negative samples were initially reported as inconclusive by the built-in software. The spectral assessment showed high selectivity for Raman peaks at 1,712 (cocaine base) and 1,716 cm -1 (cocaine HCl). Combined PLS-R and PLS-DA models using these features confirmed and further improved instrument performance. This study scientifically assessed the performance of a commercial Raman spectrometer, providing useful insight on its applicability for both presumptive detection and legally valid evidence of cocaine presence for law enforcement., (© 2020 The Authors. Drug Testing and Analysis published by John Wiley & Sons Ltd.)

On-scene drug detection is an increasingly significant challenge due to the fast-changing drug market as well as the risk of exposure to potent drug substances. Conventional colorimetric cocaine tests involve handling of the unknown material and are prone to false-positive reactions on common pharmaceuticals used as cutting agents. This study demonstrates the novel application of 740-1070 nm small-wavelength-range near-infrared (NIR) spectroscopy to confidently detect cocaine in case samples. Multistage machine learning algorithms are used to exploit the limited spectral features and predict not only the presence of cocaine but also the concentration and sample composition. A model based on more than 10,000 spectra from case samples yielded 97% true-positive and 98% true-negative results. The practical applicability is shown in more than 100 case samples not included in the model design. One of the most exciting aspects of this on-scene approach is that the model can almost instantly adapt to changes in the illicit-drug market by updating metadata with results from subsequent confirmatory laboratory analyses. These results demonstrate that advanced machine learning strategies applied on limited-range NIR spectra from economic handheld sensors can be a valuable procedure for rapid on-site detection of illicit substances by investigating officers. In addition to forensics, this interesting approach could be beneficial for screening and classification applications in the pharmaceutical, food-safety, and environmental domains., (© 2020 The Authors. Drug Testing and Analysis published by John Wiley & Sons Ltd.)

While hair analysis is important and accepted in forensic applications, fundamental knowledge gaps still exist, exacerbated by a lack of knowledge of the incorporation mechanisms of substances into hair. The influence of the hair sampling location on the head on ethyl glucuronide (EtG) and cocaine concentrations was investigated by measuring the complete scalp hair of 14 (2 EtG, 4 cocaine, 8 both EtG and cocaine) study participants in a grid pattern for EtG, drugs of abuse, and benzodiazepines. Head skin perfusion and sweating rates were investigated to rationalize the concentration differences. For EtG, ratios between maximum and minimum concentrations on the scalp ranged from 2.5 to 7.1 (mean 4.4). For cocaine, the ratios ranged from 2.8 to 105 (mean 17.6). EtG concentrations were often highest at the vertex, but the distribution was strongly participant dependent. Cocaine and its metabolites showed the lowest concentrations at the vertex and the highest on the periphery, especially at the forehead. These differences led to hair from some head parts being clearly above conventional cut-offs and others clearly below. In addition to EtG and cocaine, the distributions of 24 other drugs of abuse and benzodiazepines/z-substances and metabolites are described. No clear pattern was observed for the head skin perfusion. Sweating rate measurements revealed higher sweating rates on the periphery of the haircut. Therefore, sweat could be a main incorporation route for cocaine. Concentration differences can lead to different interpretations depending on the sampling site. Therefore, the results are highly relevant for routine forensic hair analysis., (© 2019 John Wiley & Sons, Ltd.)

The effectiveness of decontamination procedures used for the removal of external drug contamination in forensic hair analysis is an ongoing debate. This investigation evaluated wash methods complying with Society of Hair Testing (SoHT) guidelines and their capacity to remove cocaine (COC) and methamphetamine (MA) from artificially contaminated hair. The most effective decontamination method was determined using a systematic approach, involving (1) an initial washing solvent screen, (2) optimization of wash duration, (3) comparison of sequential wash methods, and (4) reanalysis of clinical hair samples. For analysis, hair was subjected to micro-pulverized methanolic extraction prior to quantitation by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Methanol (MeOH) and 0.1 M phosphate buffer (pH 6) were the most effective organic and aqueous solvents, respectively, removing 28%-38% of COC and 16%-31% of MA. Wash durations longer than 30-60 minutes did not remove additional amounts, and a more efficient sequential wash method was subsequently developed. Despite this, the interpretation of reportable results relative to the SoHT cut-off levels was unchanged for most clinical hair samples reanalyzed after washing by agitation for 30 minutes with MeOH. These findings highlight the inability of decontamination solvents to completely remove external COC and MA contamination from hair, including wash methods adhering to SoHT guidelines., (© 2019 John Wiley & Sons, Ltd.)

This work provides a new analytical method for the determination of cocaine, its metabolites benzoylecgonine and cocaethylene, the pyrolytic products anhydroecgonine and anhydroecgonine methyl ester, and the pharmaceutical levamisole in wastewater. Samples were solid-phase extracted and extracts analyzed by liquid chromatography-tandem mass spectrometry using, for the first time in the illicit drug field, a stationary phase that combines reversed-phase and weak cation-exchange functionalities. The overall method performance was satisfactory, with limits of detection below 1 ng/L, relative standard deviations below 21%, and percentages of recovery between 93% and 121%. Analysis of 24-hour composite raw wastewater samples collected in Santiago de Compostela (Spain) and Brasilia (Brazil) highlighted benzoylecgonine as the compound showing the highest population-normalized mass loads (300-1000 mg/day/1000 inhabitants). In Brasilia, cocaine and levamisole loads underwent an upsurge on Sunday, indicating a high consumption, and likely a direct disposal, of cocaine powder on this day. Conversely, the pyrolytic product resulting from the smoke of crack, anhydroecgonine methyl ester, and its metabolite anhydroecgonine were relatively stable over the four days, agreeing with a non-recreational-associated use of crack., (© 2019 John Wiley & Sons, Ltd.)

Recent studies indicate that not only the anthelminthic levamisole but also the racemate tetramisole (R-/S-phenyltetraimidazothiazole, PTHIT) was found as an adulterant for cocaine. We herein report on the investigation of the prevalence of PTHIT among cocaine-positive hair samples and the discrimination of the presence of its stereoisomers levamisole and dexamisole. Cocaine-positive hair samples were collected in a forensic context in 2015 and mainly 2017 (n = 724). Cocaine and PTHIT concentrations have been determined by achiral liquid chromatography-tandem mass spectrometry (LC-MS/MS). For distinction of levamisole/dexamisole chiral LC-MS/MS was performed. Cocaine hair concentrations ranged from 500 (cut-off) to approximately 800 000 pg/mg. The study demonstrates a strong prevalence of PTHIT in cocaine users' hair (87%, n = 627). PTHIT hair concentrations ranged from below LLOQ 3.5 to approximately 61 000 pg/mg (median: 260 pg/mg). Surprisingly, enantiomeric ratios of levamisole/dexamisole ranged from 0.17 to 1.34 (median: 0.63). Therefore, PTHIT-adulterated street cocaine samples (n = 24) seized between 2013 and 2016 were tested. Samples mainly contained racemic tetramisole (87.5%), only one sample contained levamisole only and two samples contained non-racemic PTHIT. Our experiments suggest that the presence of tetramisole in biological samples may have hitherto been underestimated. Most probably higher dexamisole than levamisole concentrations in hair specimens arise from stereoselective metabolism and/or elimination. This is particularly important in light of the different pharmacological activities of the two enantiomers and potentially different adverse effects. Toxicological interpretations in intoxication cases with adulterated cocaine should not only consider levamisole but also tetramisole and terminology in scientific contributions should be used accordingly., (© 2018 John Wiley & Sons, Ltd.)

Quick but accurate testing and on-the-spot monitoring of cocaine in oral fluids and urine continues to be an important toxicological issue. In terms of drug testing, a number of devices have been introduced into the market in recent decades, notably for workplace inspection or roadside testing. However, these systems do not always fulfill the requirements in terms of reliability, especially when low cut-off levels are required. With respect to surface water, the presence of anthropogenic small organic molecules such as prescription and over-the-counter pharmaceuticals as well as illicit drugs like cannabinoids, heroin, or cocaine, has become a challenge for scientists to develop new analytical tools for screening and on-site analysis because many of them serve as markers for anthropogenic input and consumer behavior. Here, a modular approach for the detection of cocaine is presented, integrating an electrochemical enzyme-linked immunosorbent assay (ELISA) performed on antibody-grafted magnetic beads in a hybrid microfluidic sensor utilizing flexible tubing, static chip and screen-printed electrode (SPE) elements for incubation, recognition, and cyclic voltammetry measurements. A linear response of the sensor vs. the logarithm of cocaine concentration was obtained with a limit of detection of 0.15 ng/L. Within an overall assay time of 25 minutes, concentrations down to 1 ng/L could be reliably determined in water, oral fluids, and urine, the system possessing a dynamic working range up to 1 mg/L., (© 2018 John Wiley & Sons, Ltd.)

Large quantities of illicit drugs are frequently seized by law enforcement. In such cases, a representative number of samples needs to be quickly examined prior to destruction. No procedure has yet been set up which rapidly provides information regarding the homogeneity of the samples, the presence of controlled substances, and the degree of purity. This study establishes a protocol for fast analysis of cocaine and its most common cutting agent, levamisole, in large seizures. The protocol is based on a hypergeometric sampling approach combined with Fourier-transform infrared (FTIR) spectrometry and support vector machines (SVM) algorithms as analysis methods. To demonstrate the practical use of this approach, 5 large cocaine seizures (consisting between 45 and 85 units) were analysed simultaneously with gas chromatography-mass spectrometry (GC-MS), gas chromatography-flame ionisation detector (GC-FID), and a portable FTIR spectrometer using attenuated total reflectance (ATR) sampling combined with SVM models. According to the hypergeometric sampling plan of the guidelines of the Drugs Working Group (DWG) of the European Network of Forensic Science Institutes (ENFSI), the required number of subsamples ranged between 19 and 23. Considering the identification analyses, the SVM models detected cocaine and levamisole in all subsamples of Cases 1 to 5 (100% correct classification), which was confirmed by GC-MS analysis. Considering the quantification analyses, the SVM models were able to estimate the cocaine and levamisole content in each subsample, compared to GC-FID data. The developed strategy is easy, cost effective, and provides immediate information about both the presence and concentration of cocaine and levamisole. By using this new strategy, the number of confirmation analyses with laborious and expensive chromatographic techniques could be significantly reduced., (Copyright © 2018 John Wiley & Sons, Ltd.)

Harm reduction services, including needle-exchange programmes, have been implemented in Switzerland for over 20 years. Their main aim is to lessen the negative social and/or physical consequences associated with illicit drug consumption and, therefore, improve prevention messages. To this end, knowledge of illicit drug consumption practices is necessary. Periodic self-report surveys are the primary source of data for monitoring drug users' behaviour. Analysis of residual content of used syringes can bring further and objective knowledge about consumed products through analytically confirmed data. Used syringes were sampled in 2 syringe-exchange facilities in Lausanne. These structures are a bus where the users bring back their syringes (ABS) and an automatic injecting kit dispenser (AIKD). Once syringes were collected, a validated gas chromatography-mass spectrometry (GC-MS) method was implemented in order to detect drugs (licit or illicit) contained in the residual content of used syringes. Cocaine was the most common drug detected alone (39% in ABS and 31% in AIKD), followed by the simultaneous detection of heroin and cocaine (12% and 17%) and heroin and midazolam (12% and 17%). The differences between the illicit drugs distribution of used syringes collected in AIKD and ABS were not statistically significant. Analysis of residual content of used syringes as a monitoring tool is an original approach that has already led to a better understanding of the habits of drug-injection users. Over the long term, this approach is a powerful tool to track and detect new consumption practices in a quasi-real-time., (Copyright © 2017 John Wiley & Sons, Ltd.)

Cocaine trafficking in the form of textile impregnation is routinely encountered as a concealment method. Raman spectroscopy has been a popular and successful testing method used for in situ screening of cocaine in textiles and other matrices. Quantitative analysis of cocaine in these matrices using Raman spectroscopy has not been reported to date. This study aimed to develop a simple Raman method for quantifying cocaine using atropine as the model analogue in various types of textiles. Textiles were impregnated with solutions of atropine in methanol. The impregnated atropine was extracted using less hazardous acidified water with the addition of potassium thiocyanate (KSCN) as an internal standard for Raman analysis. Despite the presence of background matrix signals arising from the textiles, the cocaine analogue could easily be identified by its characteristic Raman bands. The successful use of KSCN normalised the analyte signal response due to different textile matrix background interferences and thus removed the need for a matrix-matched calibration. The method was linear over a concentration range of 6.25-37.5 mg/cm 2 with a coefficient of determination (R 2 ) at 0.975 and acceptable precision and accuracy. A simple and accurate Raman spectroscopy method for the analysis and quantification of a cocaine analogue impregnated in textiles has been developed and validated for the first time. This proof-of-concept study has demonstrated that atropine can act as an ideal model compound to study the problem of cocaine impregnation in textile. The method has the potential to be further developed and implemented in real world forensic cases., (Copyright © 2017 John Wiley & Sons, Ltd.)

Although hair is widely used to identify drug use, there is a risk of false positives due to environmental contamination. This especially applies to cocaine (COC). Several strategies such as detection of norcocaine (NCOC) or cocaethylene, metabolite concentration ratios or intricate washing procedures have been proposed to differentiate actual use from contamination. The aim of the present study was to identify hydroxy metabolites of COC in hair specimens, thus enabling unambiguous prove of ingestion. A suspect screening of 41 COC-positive samples for these compounds was performed by liquid chromatography-quadrupole time of flight-mass spectrometry (LC-QTOF-MS). Once identified, mass transitions for o-, p- and m-isomers of hydroxy COC as well as p- and m-isomers of hydroxy benzoylecgonine (BE) and hydroxy NCOC were introduced into a routine procedure for testing drugs of abuse in hair by liquid chromatography-tandem mass spectrometry (LC-MS/MS) which was applied to 576 hair samples. Hydroxy metabolites were present in 92.2% of COC-positive hair samples; their detection rate exceeded that of cocaethylene and NCOC. Moreover, p-OH-BE, m-OH-BE as well as p-OH-NCOC and m-OH-NCOC have been identified for the first time in COC-positive hair specimens. Hydroxy cocainics could be detected in samples having a negative conclusion on drug use applying hitherto established criteria. We suggest a more conclusive interpretation outcome including detection of hydroxy metabolites into the evaluation of COC-positive hair samples., (Copyright © 2017 John Wiley & Sons, Ltd.)

Traditionally, fast screening for the presence of cocaine in unknown powders is performed by means of colour tests. The major drawbacks of these tests are subjective colour evaluation depending on the operator ('50 shades of blue') and a lack of selectivity. An alternative fast screening technique is Fourier Transform InfraRed (FTIR) spectrometry. This technique provides spectra that are difficult to interpret without specialized expertise and shows a lack of sensitivity for the detection of cocaine in mixtures. To overcome these limitations, a portable FTIR spectrometer using Attenuated Total Reflectance (ATR) sampling was combined with a multivariate technique, called Support Vector Machines (SVM). Representative street drug powders (n = 482), seized during the period January 2013 to July 2015, and reference powders (n = 33) were used to build and validate a classification model (n = 515) and a quantification model (n = 378). Both models were compared with the conventional chromatographic techniques. The SVM classification model showed a high sensitivity, specificity, and efficiency (99%). The SVM quantification model determined cocaine content with a root mean squared error of prediction (RMSEP) of 6% calculated over a wide working range from 4 to 99 w%. In conclusion, the developed models resulted in a clear output (cocaine detected or cocaine not detected) and a reliable estimation of the cocaine content in a wide variety of mixtures. The ATR-FTIR technique combined with SVM is a straightforward, user-friendly, and fast approach for routine classification and quantification of cocaine in seized powders. Copyright © 2016 John Wiley & Sons, Ltd., (Copyright © 2016 John Wiley & Sons, Ltd.)

For the first time in China, the chemical profiling of cocaine specimens was performed at the National Narcotics Laboratory. An ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry (UHPLC-QTOF-MS) method was developed and validated for simultaneous analysis of 14 cocaine alkaloids and 5 main adulterants. Among them, ecgonine methyl ester, ecgonine, benzoylecgonine, and norcocaine were identified by comparing with the standard materials; tropacocaine, 3,4,5-trimethoxycocaine, cis-/trans-cinnamoylcocaine were tentatively identified based on the exact masses of protonated molecules and product ions; six unidentified alkaloids of 182/1.47, 316/9.54, 659/9.85, 316/9.87, 420/10.34, and 420/10.85 were marked with 'extracted mass/retention time' for convenience. Minimum sample preparation and analysis time were required, which was suitable for routine analysis. Based on the semi-quantitative data set of 14 alkaloid impurities in 131 linked/unlinked cocaine samples, 50 combinations of pretreatment methods and distance/correlation measurements were tested for their potential discrimination power for cocaine profiling, and Logarithm/Pearson exhibited the best result. After hierarchical cluster analysis (HCA), 183 cocaine samples collected from 2011 to 2015 were classified into 7 major groups. Moreover, 37 groups of linked samples were found within and between provinces, which provide intelligence for the case connection and revealing of the distribution networks. Our results highlighted the practical utilities of drug profiling, especially to support the investigation through operational intelligence and to improve the knowledge related to the drug trafficking through strategic intelligence. Copyright © 2016 John Wiley & Sons, Ltd., (Copyright © 2016 John Wiley & Sons, Ltd.)

Drug exposure during pregnancy constitutes a major legal issue and a public health concern. Drug and metabolite determination in biological matrices from mother and newborn is an objective indication of prenatal drug exposure. However, limited data are available regarding the interpretation of these analytical results in terms of window of detection and degree of exposure. We collected paired maternal hair, meconium, placenta, and umbilical cord from 727 mother-newborn dyads. We analyzed these specimens by liquid chromatography-tandem mass spectrometry for the determination of cocaine, opioids, methadone, and amphetamines, and compared the analytical results from the four different matrices. The cases were divided in non-exposure, low, and frequent exposure, based on maternal hair concentrations and segmental analysis by trimesters. For cocaine, 62 cases tested positive in hair, 9 in meconium, 6 in placenta and 7 in umbilical cord. In the case of opioids, 14 maternal hair cases were positive, 11 meconium and umbilical cord and 9 placenta samples. For methadone, 11 cases were positive in hair, 9 in meconium and 6 in placenta and umbilical cord. For amphetamines, 18 cases were positive according to maternal hair, but all meconium, placenta, and umbilical cord tested negative. Maternal hair was the most sensitive specimen to detect drug exposure during pregnancy. Meconium, placenta, and umbilical cord tested positive if hair concentrations showed frequent drug use during the whole pregnancy, especially during the third trimester. Meconium, placenta, and umbilical cord also tested positive for morphine and metabolites, if this drug was administered during labour and delivery. Copyright © 2016 John Wiley & Sons, Ltd., (Copyright © 2016 John Wiley & Sons, Ltd.)

Collection of oral fluid (OF) is easy and non-invasive compared to the collection of urine and blood, and interest in OF for drug screening and diagnostic purposes is increasing. A high-throughput ultra-high-performance liquid chromatography-tandem mass spectrometry method for determination of 21 drugs in OF using fully automated 96-well plate supported liquid extraction for sample preparation is presented. The method contains a selection of classic drugs of abuse, including amphetamines, cocaine, cannabis, opioids, and benzodiazepines. The method was fully validated for 200 μL OF/buffer mix using an Intercept OF sampling kit; validation included linearity, sensitivity, precision, accuracy, extraction recovery, matrix effects, stability, and carry-over. Inter-assay precision (RSD) and accuracy (relative error) were <15% and 13 to 5%, respectively, for all compounds at concentrations equal to or higher than the lower limit of quantification. Extraction recoveries were between 58 and 76% (RSD < 8%), except for tetrahydrocannabinol and three 7-amino benzodiazepine metabolites with recoveries between 23 and 33% (RSD between 51 and 52 % and 11 and 25%, respectively). Ion enhancement or ion suppression effects were observed for a few compounds; however, to a large degree they were compensated for by the internal standards used. Deuterium-labelled and 13 C-labelled internal standards were used for 8 and 11 of the compounds, respectively. In a comparison between Intercept and Quantisal OF kits, better recoveries and fewer matrix effects were observed for some compounds using Quantisal. The method is sensitive and robust for its purposes and has been used successfully since February 2015 for analysis of Intercept OF samples from 2600 cases in a 12-month period. Copyright © 2016 John Wiley & Sons, Ltd., (Copyright © 2016 John Wiley & Sons, Ltd.)

Third-hand smoke is the residue remaining on surfaces during smoking events. It is composed of particles and vapours that form upon heating. The phrase 'third-hand smoke' is primarily used to describe nicotine and other chemicals from cigarettes, but any residues formed from the smoking of various substances could be classified similarly. There has been an increasing body of research on third-hand smoke from cigarettes in the last decade, but little has been done in regards to understanding the persistence of particles and vapours from illicit drugs. In this work, small samples of cocaine and methamphetamine were volatilized to produce an illicit drug smoke that was collected onto various surface materials and left exposed to ambient conditions over 672 h (four weeks). Chemical analyses by electrospray ionization-mass spectrometry of residues on silicon, plastic, laminate, and artificial leather surfaces indicated a rapid decrease in recovery of the parent molecule, with varied formation of decomposition products over the first 168 h of exposure. Measurable amounts of the parent molecule were still present after 672 h, exhibiting a strong persistence of these drugs on various household materials. This is important in a forensic science context, as third-hand smoke residues could provide a viable source of trace evidence previously not utilized. Published 2016. This article is a U.S. Government work and is in the public domain in the USA., (Published 2016. This article is a U.S. Government work and is in the public domain in the USA.)

The data collected in this study describe an initial attempt to systematically introduce the qualitative and quantitative analysis of adulterants present in seized street drugs in Italy with the aim of improving surveillance and data sharing and for this purpose, the implementation of validated and standardized procedures are essential., (Copyright © 2016 John Wiley & Sons, Ltd.)

Even though hair analysis often seems to be the best choice for retrospective monitoring of cocaine intake, differentiating between incorporated cocaine and external contamination is widely debated. In this study we report results obtained in 90 hair samples from addicts. All samples were analyzed for cocaine, benzoylecgonine, norcocaine, cocaethylene, and tropococaine by gas chromatography-mass spectrometry (GC-MS) techniques coupled with direct immersion solid-phase micro-extraction. Cocaine concentrations were stratified into three classes of usage: light (0.5-3 ng/mg), moderate (3.1-10 ng/mg) and heavy (10.1-40 ng/mg). The Substance Abuse and Mental Health Services Administration cut-off criteria for establishing active cocaine use were applied to the results. For all samples criteria were cocaine levels above 0.5 ng/mg (ranging from 1.63 to 39.29 ng/mg, mean 9.49 ng/mg), benzoylecgonine concentrations ≥ 0.05 ng/mg (ranging from 0.19 to 5.77 ng/mg, mean 1.40), and benzoylecgonine to cocaine % ratio ≥5% (from 6.43 to 26.09%). Norcocaine was present in 58.9% of samples (concentration range: 0.22-3.14 ng/mg) and was strongly predictive only of heavy cocaine use (sensitivity 100% for cocaine concentrations above 9.58 ng/mg). Twenty hair samples from moderate and heavy users tested positive for cocaethylene (concentration range: 0.22-1.98 ng/mg, mean 0.73 ng/mg). This study on hair samples with no chance of false positive cases highlights the very limited applications of testing minor cocaine metabolites for definitive proof of active cocaine consumption. © 2015 The Authors. Drug Testing and Analysis Published by John Wiley & Sons, Ltd., (© 2015 The Authors. Drug Testing and Analysis Published by John Wiley & Sons, Ltd.)

Hygrine (HYG) and cuscohygrine (CUS) are natural alkaloids of coca leaves but are not found in illicit cocaine seizures. Therefore, they were proposed as markers for coca chewing in contrast to cocaine abuse in urine and hair testing. In order to examine at which step of the illegal cocaine production these compounds are lost, coca leaves were processed according to an authentic procedure by extraction with lime and kerosene, re-extraction with sulphuric acid, and precipitation of coca paste with ammonia. Non-extracted and extracted coca leaves, acidic extract and coca paste were analyzed by gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) for cocaine, ecgonine methyl ester (EME), cinnamoylcocaine (CIN), HYG, and CUS. It follows from the results that under these conditions, HYG and CUS are extracted only to a minor extent by kerosene and are not precipitated from the acidic re-extract in the coca paste. Due to this behaviour in illegal cocaine production, they fulfil the conditions as markers for coca chewing in an optimal way. However, for unambiguous discrimination between coca chewing and cocaine abuse in human samples, additional markers of manufactured cocaine are required. Copyright © 2016 John Wiley & Sons, Ltd., (Copyright © 2016 John Wiley & Sons, Ltd.)

Drug testing is a harm reduction strategy that has been adopted by certain countries in Europe. Drug users are able to hand in their drugs voluntarily for chemical analysis of composition and dose. Drug users will be alerted about dangerous test results by the drug testing systems directly and through warning campaigns. An international collaborative effort was launched to combine data of drug testing systems, called the Trans European Drug Information (TEDI) project. Drug testing systems of Spain, Switzerland, Belgium, Austria, Portugal, and the Netherlands participated in this project. This study presents results of some of the main illicit drugs encountered: cocaine, ecstasy and amphetamine and also comments on new psychoactive substances (NPS) detected between 2008 and 2013. A total of 45 859 different drug samples were analyzed by TEDI. The drug markets of the distinct European areas showed similarities, but also some interesting differences. For instance, purity of cocaine and amphetamine powders was generally low in Austria, whilst high in Spain and the Netherlands. And the market for ecstasy showed a contrast: whereas in the Netherlands and Switzerland there was predominantly a market for ecstasy tablets, in Portugal and Spain MDMA (3,4-methylenedioxymethamphetamine) crystals were much more prevalent. Also, some NPS appearing in ecstasy seemed more specific for one country than another. In general, prevalence of NPS clearly increased between 2008 and 2013. Drug testing can be used to generate a global picture of drug markets and provides information about the pharmacological contents of drugs for the population at risk. Copyright © 2016 John Wiley & Sons, Ltd., (Copyright © 2016 John Wiley & Sons, Ltd.)

Monitoring population drug use through wastewater-based epidemiology (WBE) is a useful method to quantitatively follow trends and estimate total drug consumption in communities. Concentrations of drug biomarkers might be low in wastewater due to dilution; and therefore analysis of pooled urine (PU) is useful to detect consumed drugs and identify targets of illicit drugs use. The aims of the study were (1) to screen PU and urinated soil (US) samples collected at festivals for illicit drug excretion products using hyphenated techniques; (2) to develop and validate a hydrophilic interaction liquid chromatography - mass spectrometry / mass spectrometry (HILIC-MS/MS) method of quantifying urinary targets of identified drugs in wastewater; and (3) to conduct a 24 h stability study, using PU and US to better reflect the chemical environment for targets in wastewater. Cocaine (COC) and ecstasy-like compounds were the most frequently detected illicit drugs; an analytical method was developed to quantify their excretion products. Hydroxymethoxymethamphetamine (HMMA), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA), HMMA sulfate (HMMA-S), benzoylecgonine (BE), and cocaethylene (CE) had 85-102% of initial concentration after 8 h of incubation, whereas COC and ecgonine methyl ester (EME) had 74 and 67% after 8 h, respectively. HMMA showed a net increase during 24 h of incubation (107% ± 27, n = 8), possibly due to the cleavage of HMMA conjugates, and biotransformation of MDMA. The results suggest HMMA as analytical target for MDMA consumption in WBE, due to its stability in wastewater and its excretion as the main phase I metabolite of MDMA. Copyright © 2016 John Wiley & Sons, Ltd., (Copyright © 2016 John Wiley & Sons, Ltd.)

In a prospective sample of 80 mother-infant dyads, we investigated whether drugs of abuse in maternal hair measured during the pregnancy trimesters were also present in neonatal meconium. Principal drugs of abuse were analyzed in the three consecutive maternal hair segments and meconium samples by ultra-performance liquid chromatography tandem mass spectrometry assay. Of the 80 mothers, 32 (40%) presented one or more hair shafts with at least one of the analyzed drugs of abuse and/or its metabolites. The drug of abuse with a higher prevalence in our study population was methamphetamine: 19 mothers had methamphetamine in one or more hair segments (59.4%). The second most detected drug of abuse was cocaine; nine mothers presented cocaine in one or more hair segments (28.1%). Nineteen pregnant women consumed at least one drug of abuse during the first trimester, ten continued consuming drugs of abuse during the second trimester; and nine consumed until the end of pregnancy. Five of the nine newborns from mothers who consumed drugs during the whole pregnancy showed drugs of abuse in meconium samples. Newborns from the 23 remaining mothers with one or two hair shafts positive to drugs of abuse did not present drugs in their meconium. Indeed from these results, it seems that discontinuous and/or sporadic consumption during pregnancy could produce a negligible transplacental passage and hence negative results in meconium. Furthermore, the role of placenta in the metabolism and excretion of drugs of abuse is still to be precisely investigated. Copyright © 2015 John Wiley & Sons, Ltd., (Copyright © 2015 John Wiley & Sons, Ltd.)

Accurate on-site devices to screen for drug intake are critical for establishing whether an individual is driving under the influence of drugs (DUID); however, on-site oral fluid (OF) cocaine device performance is variable. We evaluated the performance of a newly developed benzoylecgonine (BE) test-strip for the Draeger® DrugTest 5000 device (20 µg/L cut-off) with equivalent cross reactivity for cocaine and BE. Ten cocaine users provided OF, collected with the Draeger cassette and Oral-Eze® and StatSure Saliva Sampler(TM) devices, up to 69 h following 25 mg intravenous cocaine administration. All screening results were confirmed by a validated two-dimensional-gas chromatography-mass spectrometry (2D-GC-MS) method for cocaine and/or BE. Cocaine test-strip median Tlast for screening only results was 6.5 h, and 6.5 h with Oral-Eze® and 4 h for StatSure OF confirmation for cocaine and/or BE at 1, 8, and 10 µg/L; sensitivity, specificity, and efficiency ranged from 85.5 to 100% and 83.3 to 100% for cocaine only confirmation at 8 and 10 µg/L. For the BE test-strip, median Tlast was 12.5 h for screening only and confirmation for cocaine and/or BE at all three cut-offs; sensitivity, specificity, and efficiency ranged from 85.5 to 97.5% and 78.4 to 97.4% with cocaine and/or BE confirmation at 8 and 10 µg/L cut-offs, respectively. The Draeger cocaine test-strip with cocaine only confirmation offers a useful option for monitoring the acute intoxication phase of DUID; additionally the BE test-strip with cocaine and/or BE confirmation increases the length of detection of cocaine intake for workplace drug testing, drug court, parole, pain management, drug treatment programs and both the acute cocaine intoxication and cocaine crash/fatigue phase of DUID. Copyright © 2016 John Wiley & Sons, Ltd., (Copyright © 2016 John Wiley & Sons, Ltd.)

Matrix-assisted laser desorption/ionization-mass spectrometry imaging (MALDI-MSI) for the analysis of intact hair is a powerful tool for the detection of drugs of abuse in toxicology and forensic applications. Here we present a quick, easy, and reproducible method of preparing longitudinal sections of single hairs. This method improves the accessibility of chemicals embedded in the hair matrix for molecular imaging with mass spectrometry. The images obtained from a single, sectioned hair sample show molecular distributions in the exposed medulla, cortex, and a portion of the cuticle observed as a narrow layer surrounding the cortex. Using MALDI-MS/MS imaging, the distribution of cocaine was observed throughout five longitudinally sectioned drug-user hair samples. The images showed the distribution of the product ion at m/z 182, derived from the precursor ion of cocaine at m/z 304. MetA-SIMS images of longitudinally sectioned hair samples showed a more detailed distribution of cocaine at m/z 304, benzoylecgonine the major metabolite of cocaine at m/z 290 and other drugs such as methadone which was observed at m/z 310. Chronological information of drug intake can be obtained more sensitively. The chronological detail is in hours rather than months, which is of great interest in clinical as well as forensic applications., (Copyright © 2015 John Wiley & Sons, Ltd.)

Desorption electrospray ionization - mass spectrometry (DESI-MS) is a useful technique for the qualitative analysis of compounds found in seized drug material. In this study, DESI-MS was utilized in the screening analysis of illicit cocaine samples. The technique was also applied to the geographical origin determination of these samples. The limit of detection was determined to be 24.3 µg (or 3.47 µg/mm(2) ) and the analysis time was less than 1 minute per sample. The intra-day and inter-day precision for the detection of cocaine was 11 % and 42 %, respectively; therefore the quantitative data provided by DESI-MS was limited in its use for accurate determination of cocaine concentration in a sample. Using the quadrupole time-of-flight (QTOF) mass spectrometer, the presence of cocaine and impurities detected were confirmed by accurate tandem MS data. The qualitative chemical profiles obtained using DESI-MS were compared to two popular analysis techniques, GC-MS and LC-MS. The effects of a range of adulterants including caffeine, procaine, levamisole, lignocaine, paracetamol, and atropine on the detectability of cocaine were also investigated. It was found that the addition of these adulterants in a cocaine sample did not prevent the detection of the analyte itself (there was slight enhancement in some samples), which was useful in drug detection. The detection of truxillines in the seized samples by DESI-MS aided in the preliminary determination of geographical origin, i.e., Bolivian, Peruvian or Colombian leaf origin. The application of DESI-MS to the qualitative analysis and screening of seized cocaine samples demonstrates the potential and applicability of the technique to the fast chemical profiling of illicit samples., (Copyright © 2014 John Wiley & Sons, Ltd.)

Workplace Drug Testing (WDT) in Italy includes two levels of monitoring: a first stage concerning drug testing on urine samples and a second involving both urine and hair analysis. The second stage is performed only on workers who tested positive at the first level. We analyzed urine and hair specimens from 120 workers undergoing second-level testing between 2009 and 2012. Eighty percent of them had tested positive for cannabinoids during the first level analysis, and 15.8% for cocaine. Both urine and hair samples were analyzed in order to find the following drugs of abuse: amphetamines, buprenorphine, cannabinoids, cocaine, ecstasy, methadone, and opiates. Urine analyses were performed by immunological screening (EMIT); urine confirmatory tests and hair analyses were performed by gas chromatography-mass spectrometry (GC-MS). As regards second-stage testing on urine samples, 71.2% of workers were always negative, whereas 23.9% tested positive at least once for cannabinoids and 2.5% for cocaine. Hair analyses produced surprising results: 61.9% of hair samples tested negative, only 6.2% tested positive for cannabinoids, whereas 28.8% tested positive for cocaine. These findings confirm that second-level surveillance of WDT, which includes hair analysis, is very effective because it highlights drug intake - sometimes heavy - that cannot be revealed only through urine analyses. The employees for whom drug addiction is proved can begin rehabilitation, while keeping their job. Eventually, our results confirmed the widespread and undeclared use of cocaine in Italy., (Copyright © 2014 John Wiley & Sons, Ltd.)

The chemical composition of a black powder confiscated by German customs was elucidated. Black powders are occasionally used as a 'transporter' for cocaine and are obviously especially designed to cloak the presence of the drug. The material consisting of cocaine, copper, iron, thiocyanate, and graphite was approached by analytical tools and chemical modelling. Graphite is added to the material probably with the intention of masking the typical infrared (IR) fingerprints of cocaine and can be clearly detected by powder X-ray diffraction (XRD) and Raman spectroscopy. Cu(2+) and NCS(-) ions, when carefully reacted with cocaine hydrochloride, form the novel compound (CocH)2 [Cu(NCS)4 ] (CocH(+)  = protonated cocaine), which has been characterised by single crystal XRD, IR, NMR, UV/Vis absorption and EPR spectroscopy. Based on some further experiments the assumed composition of the original black powder is discussed., (Copyright © 2014 John Wiley & Sons, Ltd.)

Cosmetic hair treatments have been referred to as 'the pitfall' of hair analysis. However, most cosmetic treatments, when applied to the hair as instructed by the product vendors, do not interfere with analysis, provided such treatments can be identified by the laboratory and the samples analyzed and reported appropriately for the condition of the hair. This paper provides methods for identifying damaged or porous hair samples using digestion rates of hair in dithiothreitol with and without proteinase K, as well as a protein measurement method applied to dithiothreitol-digested samples. Extremely damaged samples may be unsuitable for analysis. Aggressive and extended aqueous washing of hair samples is a proven method for removing or identifying externally derived drug contamination of hair. In addition to this wash procedure, we have developed an alternative wash procedure using 90% ethanol for washing damaged or porous hair. The procedure, like the aqueous wash procedure, requires analysis of the last of five washes to evaluate the effectiveness of the washing procedure. This evaluation, termed the Wash Criterion, is derived from studies of the kinetics of washing of hair samples that have been experimentally contaminated and of hair from drug users. To study decontamination methods, in vitro contaminated drug-negative hair samples were washed by both the aqueous buffer method and a 90% ethanol method. Analysis of cocaine and methamphetamine was by liquid chromatography-tandem mass spectrometry (LC/MS/MS). Porous hair samples from drug users, when washed in 90% ethanol, pass the wash criterion although they may fail the aqueous wash criterion. Those samples that fail both the ethanolic and aqueous wash criterion are not reported as positive for ingestion. Similar ratios of the metabolite amphetamine relative to methamphetamine in the last wash and the hair is an additional criterion for assessing contamination vs. ingestion of methamphetamine., (Copyright © 2014 John Wiley & Sons, Ltd.)

It is possible for hair to be externally contaminated by drugs like cannabis or cocaine, which are smoked or snorted. Three steps are commonly employed to minimize the chance of external contamination causing misinterpretation of the results of a hair test. The first consists of decontamination of hair samples by washing the hair before analysis, the second is the use of cut-off levels, and the third is the detection of both the parent drugs and appropriate levels of their metabolite(s) in the hair sample. We propose an additional step for the assessment of drug use using hair samples combined with decontamination data. Hair samples from 186 drug users were analyzed along with their wash residues by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The results of the hair analysis of the 140 samples for cocaine showed that 85.5% (N=89) of the samples passed 'cocaine use' criteria for metabolites ratios and 12.5% (N=13) for wash residue criteria (<10% of cocaine in the wash residue) leading to conclusive interpretation. Only two cases (1.9%) had an uncertain conclusion of drug consumption because cocaine levels in the wash residue were >10% of the levels in the hair. The results of the cannabis set of samples (N=46) were not as clear-cut, as a comparatively large number of samples (15.2%) had relatively high levels of THC in the wash residues. To use this approach, it is important that laboratories testing drugs in hair samples can demonstrate that the method utilized does not generate significant levels of the cocaine metabolites., (Copyright © 2014 John Wiley & Sons, Ltd.)

Clinical studies examining performance of fatty acid ethyl esters (FAEE) and ethyl glucuronide (EtG) in identifying excessive alcohol consumption have been primarily conducted in male populations. An impact of hair cosmetics in producing both false-negative EtG results and false-positive FAEE results has been demonstrated, suggesting a possible bias in female populations. This study evaluates FAEE-positive hair samples (>0.50 ng/mg) from n = 199 female and n = 73 male subjects for EtG. Higher FAEE/EtG concordance was observed amongst male over female subjects. Performance of multiple proposed EtG cut-off levels were assessed; amongst female samples, FAEE/EtG concordance was 36.2% (30 pg/mg), 36.7% (27 pg/mg), and 43.7% (20 pg/mg). Non-coloured hair demonstrated a two-fold increase in concordance (41.8 v. 20.8%) over coloured hair in the female cohort. FAEE levels did not differ between male and female subjects; however they were lower in coloured samples (p = 0.046). EtG was lower in female subjects (p = 0.019) and coloured samples (p = 0.026). A total of n = 111 female samples were discordant. Amongst discordant samples (EtG-negative), 26% had evidence of recent alcohol use including consultation histories (n = 20) and detectable cocaethylene (n = 9); 29% of discordant samples were coloured. False-negative risk with ethyl glucuronide analysis in females was mediated by cosmetic colouring. These findings suggest that combined analysis of FAEE and EtG is optimal when assessing a female population and an EtG cut-off of 20 pg/mg is warranted when using combined analysis. While concordant FAEE/EtG-positive findings constitute clear evidence, discordant FAEE/EtG findings should still be considered suggestive evidence of chronic excessive alcohol consumption., (Copyright © 2014 John Wiley & Sons, Ltd.)

The drug content of hair may be affected by washing, chemical or thermal treatments, the use of cosmetics, or exposure to the environment. Knowledge concerning the effect of natural or artificial light on drug content in hair can be helpful to the forensic toxicologist, in particular when investigating drug concentrations above or below pre-determined cut-offs. The photodegradation of methadone and its metabolite, 2-ethyl-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP) was studied in authentic positive hair samples by comparing drug concentrations determined by liquid chromatrography-high resolution mass spectrometry before and after exposure to UVB light (in vivo study). The same approach was applied in order to investigate the light sensitivity of opiates (6-monoacetylmorphine and morphine) and cocainics (cocaine and benzoylecgonine) in true positive hair. The yields of photodegradation were calculated for each drug class in eight different positive hair samples irradiated by UVB at 300 J/cm(2) obtaining averages, ranges and standard deviations. In parallel, the photostability of all the compounds as 10(-5) -10(-4)  M standard solutions in methanol were examined by means of UVB light irradiation in the range 0-100 J/cm(2) followed by UV/Vis spectroscopic analysis and direct infusion electrospray ionization-high resolution mass spectrometry (in vitro study). In hair, methadone was shown to be significantly affected by light (photodegradation of 55% on average), while its metabolite EDDP proved to be more photostable (17%). 6-monoacetylmorphine, morphine, benzoylecgonine, and cocaine were more photostable than methadone in vivo (on average, 21%, 17%, 20%, and 11% of degradation, respectively). When irradiated in standard solutions, the target molecules exhibited a larger photodegradation than in vivo with the exception of cocaine (photodegradation for methadone up to 70%, 6-monoacetylmorphine and morphine up to 90%, benzoylecgonine up to 67%, cocaine up to 15%). Some factors possibly affecting the yields of photodegradation in hair and partially explaining the differences observed between the in vivo and the in vitro studies were also investigated, such as the colour of hair (the role of melanin) and the integrity of the keratin matrix., (Copyright © 2014 John Wiley & Sons, Ltd.)

Wastewater analysis has the potential to provide objective and timely data on population drug consumption, but some crucial factors such as pre-analysis drug loss during sample storage and filtration could affect the accuracy and reliability of the method, and these uncertainties have yet to be fully assessed. This study was designed to evaluate analyte stability in wastewater stored under different conditions with the aim of optimizing the sample storage procedures for future studies. It also investigated whether there is significant analyte loss during filtration before sample extraction and storage after that. The studied substances and metabolites were: cotinine, cocaine and its metabolite benzoylecgonine, phenethylamines amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), opioids including codeine, methadone, 6-monoacetylmorphine (MAM) and morphine. In most situations, storing samples at 4 °C is sufficient to stabilize analytes for at least 2 weeks, and refrigeration is unnecessary during sample transportation within 3 days. However, additional measures need to be taken if unstable analytes such as cocaine and MAM are to be analyzed. No significant analyte loss was observed in the filtration process or in reconstituted extract stored at 4 °C or -20 °C for 2 weeks. By choosing stable analytes and proper storage conditions, wastewater analysis has the potential to provide accurate data for estimation of community drug use., (Copyright © 2012 John Wiley & Sons, Ltd.)

In a preliminary test, four single hairs of a drug abuser were analyzed for the presence of drugs by MALDI Fourier transform mass spectrometry (MALDI-FTMS). Washed hair strains were directly fixed on a sample plate using pressure stable, double-sided adhesive tape; α-cyano-4-hydroxycinnamic acid matrix was manually spotted onto the hair strains. FTMS full scans were obtained moving from the hair root region towards the hair tip. Cocaine (accurate m/z ratio 304.15433) was identified mostly from the root of the hair and then later again towards the hair tip. This was confirmed by analysis of a second hair. Additionally cocaine metabolites with m/z ratio 290.13868 (benzoylecgonine), and m/z 318.16998 (cocaethylene) were detected for plausibility control. Using the MALDI technique, time-related information was obtained concerning the behavioural pattern of the consumer with high resolution compared to conventional procedures. However, in two hairs of the same individual which were analyzed under the same conditions, negative results were achieved. These preliminary results confirm the applicability of MALDI-MS for the determination of drugs and pharmaceuticals in hair samples being useful in forensic toxicology. The high chronological resolution allows an enhanced interpretation concerning the periods of drug administration. However, the negative results with two negative hairs have also demonstrated that hair analysis of single hairs can lead to misinterpretation. Different growth rates have to be considered, and particularly the phenomenon of different growth phases (anagen, catagen, telogen) require attention., (Copyright © 2013 John Wiley & Sons, Ltd.)

The consumption of drugs is of great concern worldwide. Various drug tests for humans have been developed but there is no compact and easy-to-use test device available yet for direct semi-quantitative drug testing in the field. We suggest using attenuated total reflection (ATR) infrared spectroscopy as a sensing method to analyze human saliva samples with respect to drugs. In this paper, we present ATR spectra in the infrared range between 2300 and 900 cm(-1) as a first step towards such a device. We emphasize the common drug cocaine and its metabolites and investigate the problems of spectral interferences of selected diluents, masking agents, common medication, and soft drinks. Furthermore, spectra of saliva samples are recorded and a time-dependent change of the spectral signatures after alcohol consumption is presented. To the best of our knowledge, it is the first time that not only spectra of the drug of interest (cocaine) dissolved in water and in saliva but also spectra of interfering compounds possibly present in the saliva sample of a tested subject are discussed. This paper presents the most appropriate spectral range for strong cocaine absorption (including its metabolites) and minimum interference by the investigated substances. This spectral window is found to be between 1800 and 1710 cm(-1). In addition, we demonstrate the feasibility to identify cocaine in saliva at a concentration of 0.020 mg/ml with IR-ATR-spectroscopy without any separation or extraction procedures. For example, this technique could also be applied for drug detection in waste water., (Copyright © 2011 John Wiley & Sons, Ltd.)

3β-(4-Fluorobenzoyloxy)tropane (3β-FBT, fluorotropacocaine) was first reported by Finnish authorities to the European Monitoring Centre for Drugs and Drug Addiction (EMCDDA) via the Early Warning System (EWS) in 2008 and our own laboratory tentatively identified it in 2010 in several products purchased from head shops. Very little is known about this cocaine-like drug and, as no reference standards were available, we have synthesized and characterized both 3β-FBT and its 3α isomer for use as reference standards. The two compounds are separable by gas chromatography (GC) but their electron-impact (EI) mass spectra were found to be almost identical. ¹⁹F NMR spectroscopy was also found to be a useful technique for distinguishing the two isomers., (Copyright © 2011 John Wiley & Sons, Ltd.)

Recently, a number of cases of smuggling dissolved cocaine in wine bottles have been reported. The aim of the present study was to determine whether cocaine dissolved in wine can be detected by proton magnetic resonance spectroscopy ((1) H MRS) on a standard clinical MR scanner, in intact (i.e. unopened) wine bottles. (1) H MRS experiments were performed with a 3 Tesla clinical scanner on wine phantoms with or without cocaine contamination. The aromatic protons of cocaine displayed resonance peaks in the 7-8 ppm region of the spectrum, where no overlapping resonances of wine were present. Additional cocaine resonances were detected in the 2-3 ppm region of the spectrum, between the resonances of ethanol and other wine constituents. Detection of cocaine in wine (at 5 mM, i.e. ∼1.5 g/L) was feasible in a scan time of 1 min. We conclude that dissolved cocaine can be detected in intact wine bottles, on a standard clinical MR scanner. Thus, (1) H MRS is the technique of choice to examine this type of suspicious cargo, since it allows for a non-destructive and rapid content characterization., (Copyright © 2010 John Wiley & Sons, Ltd.)

The Ministry of Health in the Netherlands has made illicit drug testing for drug users possible since the 1990s, in order to prevent serious health hazards associated with unexpected dangerous substances. This system of illicit drug testing is called the Drug Information and Monitoring System (DIMS). In nearly two decades, more than 100 000 drug samples have been handed in at DIMS testing facilities. This review describes the DIMS methodology and overviews results of the three main psychostimulant drug markets that have been monitored, i.e. ecstasy, amphetamine (speed), and cocaine. Additionally, monitoring results of hallucinogens are also described for the first time. For comparison, alternative international monitoring systems are described briefly alongside some of their results. Finally, drug monitoring is discussed from the perspectives of policy, prevention, and the drug users themselves., (Copyright © 2011 John Wiley & Sons, Ltd.)

Recently, cocaine has been concealed by dissolving it in alcohol and then transporting it in solution through ports and airports. At the present time it is very difficult to detect cocaine in this form in these environments. However, it has been shown that Raman spectroscopy can successfully detect the presence of these drugs without removing specimens from their containers. Using two portable 785 nm instruments and a 1064 nm laboratory-based instrument, several common containers used in smuggling were analyzed with varying concentrations of cocaine in ethanol solutions. The presence of cocaine is detectable to about 6% w/v in most containers. Green glass presents a problem at 785 nm due to fluorescence but by switching to 1064 nm this can be removed. To apply this technique to real samples as met within law enforcement scenarios, cocaine was dissolved in a selection of dark and white rums including Lamb's Navy Rum(™) , Brugal Añejo(™) , Bacardi(™) and Captain Morgan(™) ; cocaine was detected in all these rum solutions., (Copyright © 2010 John Wiley & Sons, Ltd.)