Journal Of Analytical Toxicology[JOURNAL]
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200 papers
Trends in central/peripheral ratio of fentanyl in Harris County, TX, and Orange County, CA, from 2009 to 2020.
Behnke G, Mata D, Meneses V … +2 more , Strickland EC, Gray TR
J Anal Toxicol · 2025 Feb · PMID 39605304 · Publisher ↗
Since the opioid epidemic was declared in 2017, postmortem fentanyl cases and the need for interpretation of their results have increased. Postmortem redistribution (PMR) is one of the factors to consider when interpreti...
Since the opioid epidemic was declared in 2017, postmortem fentanyl cases and the need for interpretation of their results have increased. Postmortem redistribution (PMR) is one of the factors to consider when interpreting cases. There have been several previous studies regarding fentanyl PMR; however, these studies either have small sample sizes or were conducted prior to the declaration of the opioid epidemic, which may cause conflicting results and not be reflective of current trends. This study includes fentanyl central/peripheral (C/P) blood ratios from 748 cases from both Harris County, TX, and Orange County, TX, spanning from January 2009 to June 2022. Because the data set was determined to be non-normally distributed, a Kruskal-Wallis test was used for statistical comparisons. There were statistically significant differences between epidemic cases from the Harris County Institute of Forensic Sciences and the Orange County Crime Laboratory, C/P ratios from pre-epidemic to epidemic years, and in cases where medically related administration of fentanyl was documented when compared to cases where there was no documentation of licit fentanyl use. Various factors that could impact PMR were evaluated (age, gender, polydrug use, etc.), and no clear trend or observation was made from the data. Based on the results of this study, there is still no clear indication as to what caused the increase in C/P ratios, but it may be related to an increase in illicit fentanyl use.
Postmortem distribution of MDPHP in a fatal intoxication case.
Croce EB, Dimitrova A, Di Milia MG … +5 more , Pierotti S, Arillotta D, Barbaresi M, Focardi M, Vaiano F
J Anal Toxicol · 2025 Feb · PMID 39604091 · Full text
The synthetic cathinone (SC) 3,4-methylenedioxy-α-pyrrolidinohexanophenone (MDPHP) is structurally correlated to the 3,4-methylenedioxypyrovalerone (MDPV). In recent years, the number of intoxication cases has increased...
The synthetic cathinone (SC) 3,4-methylenedioxy-α-pyrrolidinohexanophenone (MDPHP) is structurally correlated to the 3,4-methylenedioxypyrovalerone (MDPV). In recent years, the number of intoxication cases has increased even if little is known about the pharmacokinetics properties. The Postmortem (PM) distribution of MDPHP remains largely unexplored. In these reports, MDPHP levels were quantified in blood, gastric content, and urine. This study aimed to describe the MDPHP PM distribution in several specimens, i.e. central and peripheral blood (CB and PB), right and left vitreous humor (rVH and lVH), gastric content (GCo), urine (U), and hair. The samples were collected from a cocaine-addicted 30-year-old man with a PM interval estimated in 3-4 h. Autopsy examination revealed unspecific findings, i.e. cerebral and pulmonary edema. No injection marks were observed. Toxicological analyses were performed using a multi-analytical approach: headspace gas chromatography for blood alcohol content (BAC), gas chromatography-mass spectrometry (GC-MS) for the main drugs of abuse, liquid chromatography-tandem mass spectrometry (LC-MS-MS) for benzodiazepines, and new psychoactive substances (NPS). BAC was negative (0.02 g/L). MDPHP concentrations were as follows: 1,639.99 ng/mL, CB; 1,601.90 ng/mL, PB; 12,954.13 ng/mL, U; 3,028.54 ng/mL, GCo; 1,846.45 ng/mL, rVH; 2,568.01 ng/mL, lVH; 152.38 (0.0-1.5 cm) and 451.33 (1.5-3.0 cm) ng/mg, hair. Moreover, hair segments were also positive for 3,4-dimethylmethcathinone (DMMC < limit of quantification: 0.01 ng/mg), α-PHP (0.59 ng/mg, 0.0-1.5 cm; 3.07 ng/mg, 1.5-3.0 cm), cocaine (6.58 ng/mg, 0.0-1.5 cm; 22.82 ng/mg, 1.5-3.0 cm), and benzoylecgonine (1.13 ng/mg, 0.0-1.5 cm; 4.30 ng/mg, 1.5-3.0 cm). MDPHP concentrations were significantly higher than those reported in the literature for fatal cases. For these reasons, the cause of death was probably the consumption of a lethal amount of MDPHP. Because CB and PB were similar, PM redistribution was not relevant.
LC-MS-MS confirmation of 11-nor-9-carboxy-tetrahydrocannabinol (Δ8, Δ9, Δ10) and hexahydrocannabinol metabolites in authentic urine specimens.
Patton AL, Muir L, Seither JZ … +2 more , Walterscheid JP, Karschner EL
J Anal Toxicol · 2025 Feb · PMID 39586679 · Publisher ↗
Recently, tetrahydrocannabinol (THC) isomers and other semi-synthetic cannabinoids have been introduced into the consumer market as alternatives to botanical cannabis. To assess the prevalence of these potential new anal...
Recently, tetrahydrocannabinol (THC) isomers and other semi-synthetic cannabinoids have been introduced into the consumer market as alternatives to botanical cannabis. To assess the prevalence of these potential new analytical targets, a liquid chromatography-tandem mass spectrometry confirmation method was developed for the quantitation of seven cannabinoid metabolites and the qualitative identification of four others in urine. The validated method was applied to authentic urine specimens that screened positive by immunoassay (50 ng/mL cutoff; n = 1300). The most commonly observed analytes were 11-nor-9-carboxy-Δ8-THC (Δ8- THCCOOH) and Δ9-THCCOOH, with the combination of the two being the most prominent analyte combination found. In addition to these metabolites, Δ10-THCCOOH was observed in 77 specimens. This is the first study to report Δ10-THCCOOH in authentic urine specimens, with this analyte always appearing in combination with Δ9-THCCOOH. Cross-reactivity studies were performed for (6aR,9R)-Δ10-THCCOOH using the Beckman Coulter EMIT® II Plus Cannabinoid immunoassay and demonstrated cross-reactivity equivalent to the Δ9-THCCOOH cutoff, providing added confidence in the reported prevalence and detection patterns. Additionally, 11-nor-9(R)-carboxy-hexahydrocannabinol (9(R)-HHCCOOH) was the most abundant stereoisomer (n = 12) in specimens containing HHC metabolites alone (n = 14). This is in contrast to 9(S)-HHCCOOH, which was the predominant stereoisomer in specimens containing Δ8- and/or Δ9-THCCOOH. Although HHC and Δ10-THC metabolites are emerging toxicology findings, based on these specimens collected between April 2022 and May 2024, an analytical panel containing Δ8- and Δ9-THCCOOH appears to be sufficient for revealing cannabinoid exposure within workplace monitoring and deterrence programs.
NSC-ADID position statement on performance impairment in safety-sensitive positions related to cannabis and other cannabinoids.
Corbett MR, Jones SR, Winecker RE … +1 more , Yeatman T
J Anal Toxicol · 2025 Jan · PMID 39562327 · Publisher ↗
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Optimization of a disposable pipette tips extraction for the analysis of psychoactive substances in sweat specimens using design of experiments.
Gomes NC, Bigão VLCP, de Campos EG … +3 more , Cabrices O, Costa BRBD, De Martinis BS
J Anal Toxicol · 2025 Feb · PMID 39562320 · Publisher ↗
Novel psychoactive substances continue to emerge in the marketplace and are often found as substances in traditional illicit drug materials and users are often unaware of the presence of other drugs. The proper identific...
Novel psychoactive substances continue to emerge in the marketplace and are often found as substances in traditional illicit drug materials and users are often unaware of the presence of other drugs. The proper identification and confirmation of the exposure to a drug is made possible when a biological specimen is collected and tested. Sweat is an alternative biological matrix of great interest for clinical and forensic analysis. One of the reasons is attributed to its expanded drug detection window, enabling a greater monitoring capacity, and provision of information on prospective drug use. However, the concentrations of drugs in sweat samples are often low, which requires highly sensitive and selective methods. Disposable pipette tips extraction (DPX) is a new miniaturized solid-phase extraction technique capable of efficiently extracting analytes from biological specimens, providing high recoveries, and requiring minimized solvent use. This study describes the development and optimization of two methods for the extraction of basic and neutral psychoactive substances from sweat samples using gas chromatography-mass spectrometry and Design of Experiments (DoE). The following extraction parameters were optimized by DoE techniques: sample volume, elution solvent volume, washing solvent volume, sample aspiration time, elution solvent aspiration time, and number of cycles performed, including the elution step. It was possible to design a simple extraction protocol that provided optimized recoveries for both basic and neutral compounds. The sum of analyte areas increased at a rate of 54.7% for compounds of basic character and 39.2% for compounds of neutral character. Therefore, our results were satisfactory, demonstrating that DPX can be successfully used for extracting the target drugs from sweat samples.
Validation of an LC-MS-MS method for analysis of 58 drugs of abuse in oral fluid and method comparison with an established LC-HRMS method.
Zheng Y, Axelsson MAB, Andresen Bergström M
J Anal Toxicol · 2025 Jan · PMID 39492753 · Publisher ↗
Liquid chromatography-mass spectrometry (LC-MS) methods for detection of multiple drugs of abuse (DoA) in oral fluid (OF) samples are being implemented in many clinical routine laboratories. Therefore, there is a need to...
Liquid chromatography-mass spectrometry (LC-MS) methods for detection of multiple drugs of abuse (DoA) in oral fluid (OF) samples are being implemented in many clinical routine laboratories. Therefore, there is a need to develop new multianalyte methods with simple sample pretreatment and short analysis times. The purpose of this work was to validate a method detecting 58 DoA to be used with two different OF sampling kits, the saliva collection system (SCS) from Greiner Bio-One and Quantisal from Immunalysis, using the same sample pretreatment and analytical method. A set of 110 samples collected with the SCS kit was further compared to an high-resolution mass spectrometry (LC-HRMS) method in another laboratory. The method was successfully validated, with precision and accuracy of ≤15% and z-scores of <2 for external controls. Using a sensitive LC-MS-MS instrument, the detection limits were <1 µg/l in neat oral fluid. In the comparative study between the LC-MS-MS and LC-HRMS methods using SCS samples, a good agreement was observed. Discrepancies were limited to lower concentration ranges, attributable to differences in cut-off thresholds between the methods. This work contributes to the development of LC-MS multianalyte methods for OF samples, which are suitable for clinical routine laboratories.
Method for detection of naturally occurring toxins in human urine using liquid chromatography-high-resolution mass spectrometry.
Hettick BE, Saddy A, Krajewski LC … +2 more , Johnson RC, Hamelin EI
J Anal Toxicol · 2025 Jan · PMID 39484869 · Publisher ↗
Natural toxins present an ongoing risk for human exposure that requires a rapid and accurate diagnosis for proper response. In this study, a qualitative liquid chromatography-high-resolution mass spectrometry (LC-HRMS) m...
Natural toxins present an ongoing risk for human exposure that requires a rapid and accurate diagnosis for proper response. In this study, a qualitative liquid chromatography-high-resolution mass spectrometry (LC-HRMS) method was developed and validated for the detection of a large, diverse selection of natural toxins. Data-dependent acquisition was performed to identify compounds with an in-house mass spectral library of 129 hazardous toxins that originate from plants, animals, and fungi. All 129 compounds were spiked into human urine, extracted, and evaluated for spectral library matching. Of these, 92 toxins met the quality criteria and underwent validation in urine matrix based on American National Standards Institute guidelines. A generalized workflow for method expansion was developed and enables the rapid addition of relevant compounds to the established method. This LC-HRMS method achieves efficient detection of natural toxins in urine, and the created workflow can rapidly increase compound coverage via method expansion.
Ethanol stability from 9 years of a blind quality control program in blood alcohol analysis.
Phung E, Rodgers C, Gooden A … +2 more , Stout P, Lee D
J Anal Toxicol · 2025 Jan · PMID 39484863 · Publisher ↗
A blind quality control (BQC) program in blood alcohol analysis was implemented at the Houston Forensic Science Center (HFSC) in September 2015. By mimicking authentic toxicology blood evidence, the laboratory can perfor...
A blind quality control (BQC) program in blood alcohol analysis was implemented at the Houston Forensic Science Center (HFSC) in September 2015. By mimicking authentic toxicology blood evidence, the laboratory can perform a concurrent evaluation of their technical and administrative casework procedures and test the accuracy and reliability of their volatile analysis method in a format that is blinded to the analyst. From September 2015 to November 2023, HFSC's Quality Division submitted 1228 antemortem whole-blood samples: 292 ethanol-negative samples and 936 ethanol-positive samples at 16 target concentrations (0.051, 0.080, 0.100, 0.110, 0.120, 0.130, 0.150, 0.160, 0.170, 0.180, 0.190, 0.200, 0.230, 0.240, 0.250, and 0.260 g/dL). A second, unopened blood tube in 168 of the 1228 BQCs was also analyzed after 721-1140 days: 24 ethanol-negative samples and 144 ethanol-positive samples at 5 target concentrations (0.080, 0.100, 0.130, 0.180, and 0.240 g/dL). All 316 ethanol-negative samples remained negative. After 42-758 days, the average (median, range) change in ethanol concentration of the 936 positive samples was -1.4% (-1.3%, -12.0% to +8.4%) with a statistically significant difference (P < .001) observed for the gradual decline in blood alcohol concentration (BAC) over time. The average BAC percentage differences per target concentration, ranged from -6.4% (-0.008 g/dL) to +5.7% (+0.011 g/dL), were within HFSC's current measurement uncertainty (9.4% at k = 3), showing no apparent correlation between the change in ethanol and the theoretical target concentration. As the analysis time between the two blood specimens from the same evidence kit extended, the loss in ethanol significantly increased (P < .001).
Postmortem diphenhydramine blood concentrations in children.
Wallage HR, Elliot M
J Anal Toxicol · 2025 Feb · PMID 39453751 · Publisher ↗
Diphenhydramine has been available for decades in non-prescription formulations for the treatment of allergic reactions, insomnia, and symptomology associated with colds. In addition, dimenhydrinate, a precursor to diphe...
Diphenhydramine has been available for decades in non-prescription formulations for the treatment of allergic reactions, insomnia, and symptomology associated with colds. In addition, dimenhydrinate, a precursor to diphenhydramine, is available in preparations for the treatment of nausea and vomiting. Diphenhydramine and other first-generation antihistamines are being replaced by second- and third-generation antihistamines, which are associated with fewer side effects, notably the lack of drowsiness; however, there are still a variety of therapeutic uses that have persisted in both adults and children. In this study, postmortem blood concentrations of diphenhydramine were determined, by liquid chromatography-tandem mass spectrometry, in seven children with concentrations ranging from 0.051 to 2.6 mg/l. The cause of death in two cases was attributed, at least in part, to diphenhydramine toxicity, while diphenhydramine detection in five cases was considered incidental to the cause of death.
Long-term stability of sufentanil quantified by UPLC-MS-MS in human plasma frozen for 11 years at -20°C.
Wehrfritz A, Schmidt S, Ihmsen H … +2 more , Schüttler J, Jeleazcov C
J Anal Toxicol · 2025 Jan · PMID 39417284 · Publisher ↗
The long-term stability of drug concentrations in human plasma samples, when stored under normal laboratory conditions over several years, is important for research purposes and clinical re-evaluation, and forensic toxic...
The long-term stability of drug concentrations in human plasma samples, when stored under normal laboratory conditions over several years, is important for research purposes and clinical re-evaluation, and forensic toxicology. Fifty human plasma samples from a former clinical trial were re-analyzed after storage at -20°C for 11 years. Plasma samples were extracted using solid-phase extraction. Isotope labeled sufentanil-d5 was used as internal standard. Sufentanil plasma concentrations were determined by ultra-performance liquid chromatography with gradient elution, followed by tandem mass spectrometry with electrospray ionization. The linear dynamic range was 25-2500 pg/mL, the limit of detection was 10 pg/mL, and the lower limit of quantification was 25 pg/mL. Intra- and inter-assay error did not exceed 6%. The deviation of the measured sufentanil plasma concentrations between the re-analysis and the first analysis was -63 ± 14% (mean ± SD). Therefore, sufentanil concentrations in human plasma were not stable in samples frozen at -20°C over 11 years.
Double designers: detection of bromazolam and metonitazene in postmortem casework.
Van Cleve D, Liebl M, Kazaryan A
J Anal Toxicol · 2025 Feb · PMID 39412128 · Publisher ↗
The identification of novel psychoactive substances (NPSs) in casework at the Los Angeles County Department of Medical Examiner (LACDME) is constantly evolving. The case detailed herein marks the first detection of meton...
The identification of novel psychoactive substances (NPSs) in casework at the Los Angeles County Department of Medical Examiner (LACDME) is constantly evolving. The case detailed herein marks the first detection of metonitazene (MTZ) in forensic casework at the LACDME, which occurred in August 2023. Furthermore, bromazolam was found in the decedent's system and both substances were identified in drug evidence collected at the death scene. No other drugs were detected and the manner and cause of death were determined as accidental due to effects of bromazolam and MTZ. The concentrations detected were 1.6 ng/mL and 4.4 ng/mL of MTZ in the jugular blood and femoral blood, respectively, and 93 ng/mL of bromazolam in the femoral blood. Constraints in screening techniques conducted by toxicology laboratories create challenges in which numerous NPSs available on the illicit drug market can go undetected. Even if labs detect an NPS in their screening methodology, confirmation methods might not cover every NPS, given the impracticality of labs keeping pace with validations as new NPSs emerge in casework. The significance of testing medical evidence collected at death scenes by drug chemistry analysis becomes crucial when initial toxicology results are negative. In cases where there is evidence of potential drug paraphernalia, this is especially true as it can be pivotal in determining the cause and manner of death.
Liquid-liquid extraction solvent selection for comparing illegal drugs in whole blood and dried blood spot with LC-MS-MS.
Aydoğdu M, Ertaş H, Ertaş FN … +1 more , Akgür SA
J Anal Toxicol · 2025 Jan · PMID 39366924 · Full text
This study focused on the simultaneous detection of amphetamine, 3,4-methylenedioxy methamphetamine, morphine, benzoylecgonine, and 11-nor-9-carboxy-tetrahydrocannabinol in whole blood and dried blood spot (DBS). It is a...
This study focused on the simultaneous detection of amphetamine, 3,4-methylenedioxy methamphetamine, morphine, benzoylecgonine, and 11-nor-9-carboxy-tetrahydrocannabinol in whole blood and dried blood spot (DBS). It is aimed to select a solvent mixture for liquid-liquid extraction technique employing liquid chromatography-tandem mass spectrometry (LC-MS-MS). The obtained DBS results were compared with the whole blood samples results. A simple, rapid, and reliable LC-MS-MS method was developed and validated for all analytes in whole blood and DBS. LC was performed on a Hypersil Gold C18 column with an initial gradient of 0.01% formic acid, 5 mM ammonium format buffer in water, and acetonitrile at 0.3 ml/min with 7.5 min runtime. A methanol:acetonitrile (40:60 v/v) mixture was selected for both matrices. Limit of quantitation (LOQ) values were 10-25 ng/mL; linear ranges were LOQ-500 ng/ml for all analytes; correlation coefficients were greater than 0.99, and all calibrator concentrations were within 20%. Analytical recovery in blood and DBS ranged from 84.9% to 113.2% of the expected concentration for both intra- and inter-day. Analytes were stable for 1, 10, and 30 days after three freeze/thaw cycles. It was determined that the variances of the results obtained with the two matrices in the comparison study were equal for each analyte, and the results were highly correlated (r = 0.9625). A sensitive, accurate, and reliable chromatographic method was developed to determine amphetamine, 3,4-methylenedioxy methamphetamine, morphine, benzoylecgonine, and cannabis, by performing the same preliminary steps with whole blood and dried blood spots. It was observed that the results obtained in these two matrices were compatible and interchangeable when statistically compared.
Detection of "smoke powder" etomidate and its metabolite etomidate acid in blood and urine by UHPLC-MS-MS: application in authentic cases.
Liying Z, Junbo Z, Wanting X … +4 more , Ping X, Yan S, Hejian W, Hui Y
J Anal Toxicol · 2024 Nov · PMID 39340313 · Publisher ↗
Recently, etomidate has been widely used as an alternative in illicit drug market. It is usually added to regular cigarette tobacco (commonly known as "cigarette powder") or mixed in e-cigarette oil sold through the Inte...
Recently, etomidate has been widely used as an alternative in illicit drug market. It is usually added to regular cigarette tobacco (commonly known as "cigarette powder") or mixed in e-cigarette oil sold through the Internet, retail stores, or entertainment outlets and other channels. An ultra-high performance liquid chromatography tandem mass spectrometry method was developed to quantify etomidate and etomidate acid in human blood and urine. The limit of detection (LOD) of etomidate and etomidate acid in blood is 0.5 and 2 ng/mL, respectively, and the lower limit of quantification (LLOQ) is 1 and 5 ng/mL, respectively. The LOD of etomidate and etomidate acid in urine is 1 and 2 ng/mL, respectively, and the LLOQ is 2 and 5 ng/mL, respectively. The precision, accuracy, recoveries, and matrix effects of etomidate and etomidate acid determinations in blood and urine met the requirements for methodological validation. The method was successfully applied to the identification and quantification of etomidate and etomidate acid in blood and urine of 62 forensic cases. The concentration of etomidate ranged from 1.52 to 8.41 ng/mL (positive cases, n = 5) and the concentration of etomidate acid ranged from 2.76 to 112 ng/mL (positive cases, n = 5) in blood. The concentrations of etomidate and etomidate acid in urine samples were 2.64-79,300 ng/mL (positive cases, n = 59) and 6.11-518,000 ng/mL (positive cases, n = 60), respectively. Therefore, the concentration of etomidate in blood and urine is mostly higher than that of etomidate.
The rise of bromazolam in postmortem cases from Travis County, TX, and surrounding areas: 2021 to 2023.
Ellefsen KN, Smith CR, Simmons PD … +2 more , Edelman LA, Hall BJ
J Anal Toxicol · 2025 Jan · PMID 39275788 · Publisher ↗
As novel psychoactive substances (NPSs) have continued to emerge over the past decade, NPS benzodiazepines have likewise increased in prevalence. They pose an evolving threat to public health and safety with regard to po...
As novel psychoactive substances (NPSs) have continued to emerge over the past decade, NPS benzodiazepines have likewise increased in prevalence. They pose an evolving threat to public health and safety with regard to postmortem cases, particularly when used in combination with opioids. Bromazolam was first detected in Travis County, Texas, in April 2021. Given the recent onset of the fentanyl epidemic in this region, the international rise of bromazolam, and increased reports of "benzo-dope," a retrospective study was conducted to characterize bromazolam-positive deaths in Travis County and surrounding counties from 2021 to 2023. Bromazolam was identified in 112 deaths from 2021 to 2023, accounting for 1.57% of cases submitted for toxicology testing (n = 7129). During that interval, a 7.5-fold increase in postmortem bromazolam-related drug toxicities from 2021 (n = 7) to 2023 (n = 53) was observed. Fatalities primarily occurred in men in their early 30s. Postmortem concentrations ranged from 21 to 220 ng/mL, with mean (median) concentrations of 69.4 ± 48.4 (53.5) ng/mL. Polydrug use was present in 99% of bromazolam-positive deaths with co-occurrence with other drugs and drug classes widely varying over time. Bromazolam was attributed as the sole cause of death in one case with a postmortem blood concentration of 23 ng/mL. Polydrug use in bromazolam-related drug toxicities commonly involved fentanyl (82%), methamphetamine (41%), and cocaine (28%). Similarly, cases where bromazolam was an incidental finding and noncontributory to the cause of death often involved methamphetamine (38%), alprazolam (33%), and cocaine (33%). In light of the significant increase in fentanyl-related deaths in Travis County, the increasing prevalence of bromazolam accompanying fentanyl was particularly alarming due to the heightened risk of toxicity when used in combination. Identifying and evaluating bromazolam-related deaths clarify the impact of bromazolam on this population, promote awareness, and aid in identifying meaningful harm reduction strategies to decrease bromazolam-related morbidity and mortality.
Four-year evaluation of drug-impaired driving drug concentrations.
Cieri G, Mohr ALA, Fogarty M … +2 more , Chan-Hosokawa A, Logan BK
J Anal Toxicol · 2024 Nov · PMID 39269138 · Publisher ↗
Drug-impaired driving is a significant public health and safety concern in the USA. To help assess current patterns of drug use in drivers, we evaluated 4 years of drug positivity in a large cohort of suspected impaired...
Drug-impaired driving is a significant public health and safety concern in the USA. To help assess current patterns of drug use in drivers, we evaluated 4 years of drug positivity in a large cohort of suspected impaired drivers. Samples collected between January 2017 and December 2020 were tested via a method compliant with the National Safety Council's Alcohol, Drugs, and Impairment Division's Tier I scope of recommended drugs. In 2017, NMS Labs received 17 346 driving under the influence of drugs cases, 17 471 in 2018, 19 050 in 2019, and 16 539 in 2020. The most common drug class detected was cannabinoids in ∼50% of the cases each year. The most common drugs detected over the 4 years were delta-9 tetrahydrocannabinol (delta-9 THC), ethanol, amphetamine/methamphetamine, fentanyl, and alprazolam. Delta-9 THC increased in positivity over the study, having been identified in 45% of cases in 2017, 46% in 2018, 46% in 2019, and 49% in 2020. Ethanol was found in 59% of cases in 2017, 59% in 2018, 61% in 2019, and 53% in 2020. Delta-9 THC and ethanol were the most common drug combination, found together in ∼19% of the cases every year of the study. Statistically significant increases in the average concentration of the following drugs were observed: fentanyl (5.7 ng/mL in 2017 to 9.6 ng/mL in 2020), methamphetamine (301 ng/mL in 2017 to 381 ng/mL in 2020), and delta-9-THC (6.4 ng/mL in 2017 to 7.3 ng/mL in 2020). Other findings included increases in the maximum reported concentrations between 2017 and 2020 for amphetamine (1400 to 2700 ng/mL), methamphetamine (5550 to 13 000 ng/mL), and fentanyl (56 to 310 ng/mL). Statistically significant concentration decreases were noted for several central nervous system depressants, notably prescription benzodiazepines, and several prescription narcotic analgesics.
Development and method validation of a sampling technique for a reproducible detection of synthetic cannabinoids in exhaled breath using an in vitro pig lung model.
Walle N, Doerr AA, Peters B … +5 more , Laschke MW, Menger MD, Schmidt PH, Meyer MR, Schaefer N
J Anal Toxicol · 2024 Nov · PMID 39252605 · Publisher ↗
Alternative matrices, especially exhaled breath (EB), have gained increasing attention for a few years. To interpret toxicological findings, knowledge on the toxicokinetic (TK) properties of a substance in EB is indispen...
Alternative matrices, especially exhaled breath (EB), have gained increasing attention for a few years. To interpret toxicological findings, knowledge on the toxicokinetic (TK) properties of a substance in EB is indispensable. While such data are already accessible for various drugs (e.g. Δ9-tetrahydrocannabinol), they are still not available for new psychoactive substances, particularly synthetic cannabinoids (SCs). As SCs raise a high public health concern, the aim of this study was to assess these data in future TK studies in pigs. For this purpose, an in vitro sampling technique of EB was initially developed, which is prospectively applied to anesthetized and ventilated pigs for the detection of SCs in a controlled and reproducible manner as exemplified by cumyl-5F-P7AICA. Furthermore, a method for the qualitative and quantitative detection of cumyl-5F-P7AICA in EB using glass fiber filters (GFFs) was established and fully validated. Therefore, cumyl-5F-P7AICA (0.5 mg/mL in ethanol absolute) was initially nebulized using a ventilation machine and a breathing tube, as they are also used in surgeries. The aerosol was delivered into a simulated pig lung. To collect EB, a pump was connected to that part of the breathing tube, which contains EB (expiratory limb), and sampling was performed repeatedly (n = 6) for 15 min (2 l EB/min) each using GFF. For extraction of the substance, the GFFs were macerated with acetone and the remaining experimental components were rinsed with ethanol. After sample preparation, the extracts were analyzed by liquid chromatography tandem mass spectrometry. In the complete experimental setup, about 40% of the initially nebulized cumyl-5F-P7AICA dose was found, with 3.6 ± 1.3% being detected in the GFF. Regarding the comparably high loss of substance, the open ventilation system and a conceivable adsorption of the SC in the ventilator have to be considered. However, the herein introduced approach is promising to determine the TK properties of cumyl-5F-P7AICA in EB.
Multi-class analysis of 57 drugs quantitatively in blood and qualitatively in urine by LC-MS-MS to complement comprehensive DFC, DUID, and postmortem testing.
Rodda LN, Farley M, Towler S … +2 more , Devincenzi T, Pearring S
J Anal Toxicol · 2025 Jan · PMID 39252597 · Publisher ↗
A streamlined LC-MS-MS method utilizing protein precipitation and filtration extraction was developed to consolidate analyses for drug-facilitated crimes (DFCs), postmortem (PM) investigations, and driving under the infl...
A streamlined LC-MS-MS method utilizing protein precipitation and filtration extraction was developed to consolidate analyses for drug-facilitated crimes (DFCs), postmortem (PM) investigations, and driving under the influence of drug (DUID) testing. Fifty-seven target drug and metabolite analytes eluted in <6 minutes and were compromised of gamma-hydroxybutyric acid precursors (1), hallucinogens (3), muscle relaxants (3), anticonvulsants (7), antidepressants (20), antihistamines (5), antipsychotics (11), antihypertensives and alpha-adrenergics (3), analgesics and anesthetics (3), and miscellaneous (1) in blood (quantitatively) and urine (qualitatively). Limits of detection were set to meet the more challenging sensitivity requirements for DFC and are therefore also suitable for PM investigations and other forensic casework, including DUID. Comprehensive Academy Standards Board / American National Standards Institute (ASB/ANSI) validation was performed, and applicability studies examined 72 proficiency test blood and urine samples, along with 9206 unique blood and urine samples from 5192 authentic forensic cases that resulted in 11,961 positive analytes in samples. By expanding the analytical reach across multiple drug classes through a unified approach and screening a wider number of drugs, the technique can identify substances that might have previously evaded detection, thereby enhancing laboratory efficiency by minimizing the need for multiple tests. When combined with a recently developed in-house method, this integrated testing strategy meets the testing requirements outlined in ASB/ANSI standards and recommendations for DFC, PM, and Tier 1 DUID analyses.
Development and validation of a simple chromatographic method to screen oral fluid samples for drugs in DUID investigations.
Sarris GG, Abbott DL, Moreno TM … +2 more , Maychack KJ, Limoges JF
J Anal Toxicol · 2024 Oct · PMID 39230975 · Publisher ↗
A simple and rapid qualitative chromatographic method with a unique extraction approach was developed and validated to screen oral fluid samples for 31 compounds in driving under the influence of drugs investigations. Th...
A simple and rapid qualitative chromatographic method with a unique extraction approach was developed and validated to screen oral fluid samples for 31 compounds in driving under the influence of drugs investigations. The scope and sensitivity of the method meets or exceeds Tier I recommendations established by the National Safety Council's Alcohol, Drugs and Impairment Division. Since this is a targeted chromatographic screen (rather than an immunoassay), cutoffs were set to match the confirmation levels in the recommendations. Sample preparation involved a single-step liquid-liquid extraction procedure, using a mixture of methyl tert-butyl ether, isopropanol, and hexane and was applied to samples collected with the Quantisal™ device. Instrument analysis was conducted by liquid chromatography-tandem mass spectrometry, using a Restek Raptor™ biphenyl column for chromatographic separations and a total run time of 8 min. Validation results met all requirements of ANSI/ASB Standard 036 (1st edition)-Standard Practices for Method Validation in Forensic Toxicology.
Assessment of postmortem urine fentanyl detection by autopsy dipstick testing in accidental overdose deaths.
Tsang A, Rodda LN
J Anal Toxicol · 2024 Nov · PMID 39230968 · Publisher ↗
Accidental overdose cases continue to rise due to the opioid epidemic in the USA, namely, the widespread availability and use of fentanyl. Medical examiners and coroners across the country have been subsequently burdened...
Accidental overdose cases continue to rise due to the opioid epidemic in the USA, namely, the widespread availability and use of fentanyl. Medical examiners and coroners across the country have been subsequently burdened, and with limited resources, some seek alternative triaging processes to identify overdoses. Point-of-care urine dipstick testing at autopsy is one such idea that may be used in various ways to instigate or negate the need for an autopsy or regular forensic toxicology laboratory testing. This study investigated the frequency and estimated quantitative fentanyl and norfentanyl concentrations in the postmortem urine of fentanyl-related accidental overdose deaths, as well as the effectiveness of commercially available point-of-care urine dipstick tests based on such concentrations. A total of 1550 fentanyl-related accidental overdose cases, where both the postmortem peripheral femoral blood and urine were tested, were reviewed. Of these, using sensitive liquid chromatography-tandem mass spectrometry (LC-MS-MS) laboratory testing, 82 cases (5%) had a positive fentanyl or norfentanyl detection in the blood, while fentanyl or norfentanyl remained undetected in the urine. Furthermore, a comparison of commercially available urine dipstick test cut-offs and authentic casework with estimated urine concentrations revealed that at a fentanyl/norfentanyl cut-off level of 5 ng/mL, 19% of these fentanyl-related accidental overdoses would result in a false negative, 24% at 10 ng/mL, 25% at 20 ng/mL, 51% at 50 ng/mL, and 61% at 100 ng/mL. The study found that the use of urine dipstick tests, as a decision-maker for the initiation of further comprehensive routine toxicology laboratory testing, or to support cause and manner of death determination, leads to both false-positive and false-negative predictions in fentanyl accidental overdoses.
Identification of 5-aminometonitazene and 5-acetamidometonitazene in a postmortem case: are nitro-nitazenes unstable?
Parks C, Maskell PD, McKeown DA … +1 more , Couchman L
J Anal Toxicol · 2024 Nov · PMID 39219540 · Publisher ↗
In recent years, the use of 2-benzylbenzimidazole opioids ('nitazenes') has increased with them becoming one of the most prominent synthetic opioid subclasses of novel psychoactive substances. With the increased prevalen...
In recent years, the use of 2-benzylbenzimidazole opioids ('nitazenes') has increased with them becoming one of the most prominent synthetic opioid subclasses of novel psychoactive substances. With the increased prevalence, there is also a concern of the dangers to public health with the use of nitazenes due to their high potency especially with polypharmacy. To aid in the detection of such compounds, it is important that forensic toxicology laboratories maintain up-to-date compound libraries for drug screening methods and that sensitive analytical instrumentation is available to detect the low blood/plasma concentrations of more potent drugs. This includes not only the compounds themselves but also potential metabolites and/or degradation products. Metonitazene is a 'nitro-nitazene' with a nitro group at position 5 of the benzimidazole ring. As a nitro-nitazene, there is a potential for bacterial degradation of metonitazene to 5-aminometonitazene, as occurs with nitro-benzodiazepines. In this study, we provide evidence from a postmortem (PM) case of degradation of metonitazene in unpreserved PM blood using liquid chromatography-triple quadrupole mass spectrometry (LC-QQQ-MS), and putative identification of the degradation/metabolic products 5-aminometonitazene and 5-acetamidometonitazene by liquid chromatography-quadrupole time-of-flight mass spectrometry. The results from LC-QQQ-MS analysis indicated that there did not appear to be such degradation in preserved (fluoride/oxalate) blood. These results suggest that nitro-nitazenes may be subject to similar in vitro stability/degradation issues as nitro-benzodiazepines. These breakdown products should be added to instrument libraries to aid in the detection of the use of nitro-nitazenes, and nitro-nitazenes should be quantified in preserved blood samples where available.
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