Journal of analytical toxicology最新文献

{"title":"Green liquid-liquid microextraction for quantification of ketamine and metabolites in human urine by gas chromatography-mass spectrometry.","authors":"Hsueh-Hui Yang, Chia-Sui Kao, Ahai C Lua, Tsong-Yung Chou","doi":"10.1093/jat/bkaf022","DOIUrl":"https://doi.org/10.1093/jat/bkaf022","url":null,"abstract":"<p><p>This study aimed to develop and validate a green method for the detection of ketamine and its metabolites in human urine samples and subsequently determine which metabolite is more suitable for judgment of ketamine abuse. Ketamine and its metabolites were extracted from urine samples with 1-undecanol using liquid-liquid microextraction based on the solidification of floating organic droplet extraction. The extracts were directly analyzed using gas chromatography-mass spectrometry (GC-MS) without derivatization. The sample pretreatment procedure prior to GC-MS analysis was simple, fast, and required little solvent consumption. Parameters that affect the extraction efficiency, including pH of the urine sample and centrifugation speed, were optimized. Under the optimized conditions, the limits of detection for norketamine, dehydronorketamine, and ketamine were 1.5, 1.7 and 1.0 ng/mL, respectively. The method was used to analyze eight real urine samples from drug abusers and exhibited acceptable accuracy and precision. By analyzing real samples, this study revealed that detection of dehydronorketamine in urine samples for the judgment of ketamine abuse may be more suitable than detection of norketamine or ketamine. The method used in this study addresses the need for green analytical techniques in toxicology.</p>","PeriodicalId":14905,"journal":{"name":"Journal of analytical toxicology","volume":" ","pages":""},"PeriodicalIF":2.3,"publicationDate":"2025-03-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143605041","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Beyond the baseline: quantification of two phosphatidylethanol homologues in whole blood by LC-MS-MS and retrospective data analysis from a National Reference Laboratory.","authors":"Nicole J Mathewson, Nkemakonam C Okoye, Heather A Nelson, Vrajesh Pandya, Chad Moore, Kamisha L Johnson-Davis","doi":"10.1093/jat/bkae100","DOIUrl":"10.1093/jat/bkae100","url":null,"abstract":"<p><p>Alcohol is the most abused substance in Western society, resulting in major economic losses and negative health consequences. Therefore, there is a need for a selective and robust detection method for alcohol consumption in various clinical and forensic settings. This study aimed to validate a mass spectrometry method for quantifying phosphatidylethanol (PEth) and perform retrospective data analysis from the patient population of a national reference laboratory. Quantification of PEth in whole blood was accomplished using an LC-MS-MS assay. Isotopically labeled internal standard for the two PEth homologues was added to the whole-blood specimen, followed by protein precipitation with a mixture of acetonitrile and isopropyl alcohol. After centrifugation, an aliquot of the supernatant was buffered with ammonium acetate before LC-MS-MS analysis on an Agilent 6470 triple quadrupole mass spectrometer coupled to an Agilent 1260 Infinity II LC system. This LC-MS-MS assay was validated for clinical use in accordance with Clinical & Laboratory Standards Institute guidelines. The analytical measurement range, 10-2000 ng/mL, was linear with R2 of 0.999. The within-run and total imprecision was < 5% CV for the low (20 ng/mL), medium (200 ng/mL), and high QC (1000 ng/mL). Results from accuracy and method comparison experiments met the bias criteria of ±15%. Retrospective data analysis showed ∼27% of patients had PEth concentrations <20 ng/mL. Males and females had similar positivity rates for PEth and the positivity rate of women of reproductive age (15-44 years old) was 35% in comparison to 25% in women 45-89 years old. This study's LC-MS-MS method showed acceptable analytical performance in quantifying PEth as a sensitive and specific biomarker for evaluating alcohol consumption. Results from this study may provide an opportunity to educate women of reproductive age on drinking during pregnancy and the long-term effects of alcohol use.</p>","PeriodicalId":14905,"journal":{"name":"Journal of analytical toxicology","volume":" ","pages":"191-200"},"PeriodicalIF":2.3,"publicationDate":"2025-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11892556/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142970705","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Effects of dichloromethane, nitrate, and sulfhemoglobin-induced substances on carboxyhemoglobin detection: a comprehensive review.","authors":"Jialin Wu, Yujing Luan, Qingxia Zhang, Fanglin Wang, Yulan Rao","doi":"10.1093/jat/bkae096","DOIUrl":"10.1093/jat/bkae096","url":null,"abstract":"<p><p>Carbon monoxide (CO) is a common gaseous toxin that causes severe poisoning symptoms. Accurate detection of the formation of carboxyhemoglobin (COHb) in the blood is very important for the identification of CO poisoning. In this review, the effects of exogenous toxins, including dichloromethane (DCM), nitrite, and hydrogen sulfide, on the determination of COHb by spectrophotometry are summarized by comparing epidemiological data, case studies, and analytical methods. The mechanism of the effects of these exogenous poisons on COHb detection is described, and the extent of their influence on the clinical diagnosis and forensic identification of CO poisoning is discussed. We suggest that emergency medicine and forensic science practices need to improve the understanding of these toxins and optimize clinical diagnosis and evaluation strategies to address the effects of toxins on the determination of COHb.</p>","PeriodicalId":14905,"journal":{"name":"Journal of analytical toxicology","volume":" ","pages":"170-179"},"PeriodicalIF":2.3,"publicationDate":"2025-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142836506","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Advances in analytical methodologies for detecting novel psychoactive substances: a review.","authors":"Alex J Krotulski, Dani C Mata, Christina R Smith, Kaitlyn B Palmquist-Orlando, Celia Modell, Svante Vikingsson, Michael T Truver","doi":"10.1093/jat/bkae098","DOIUrl":"10.1093/jat/bkae098","url":null,"abstract":"<p><p>Novel psychoactive substances (NPSs) have historically been difficult compounds to analyze in forensic toxicology. The identification, detection, and quantitation of these analytes and their metabolites have been difficult due to their rapid emergence, short lifespan, and various potencies. Advancements in analytical instrumentation are fundamental to mitigating these NPS challenges by providing reliable identification and sensitivity. This review discusses the pros and cons of various analytical instruments that have played a pivotal role in NPS analysis. As analytical technology advanced, the ability to analyze for NPS became easier with high-resolution mass spectrometry (MS); however, traditional immunoassays are still beneficial for some NPS classes such as benzodiazepines. Over 200 articles from 2010-23 were reviewed, and 180 were utilized for this review. Journal articles were categorized according to the technology used during analysis: immunoassay, gas chromatography-MS, liquid chromatography-MS-low resolution, and liquid chromatography-MS-high resolution to allow for quick references based on a laboratory's technologies. Journal articles were organized in table format to outline the authors, NPS drug classes, and instrumentation used, among other important information.</p>","PeriodicalId":14905,"journal":{"name":"Journal of analytical toxicology","volume":" ","pages":"152-169"},"PeriodicalIF":2.3,"publicationDate":"2025-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142949241","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Bladder wash: a proof of concept as an alternative specimen for postmortem toxicology.","authors":"Luke N Rodda, Kylie E Candela, Amy P Hart, Ellen G Moffatt, Megan C Farley, Sue Pearring, Karen S Scott","doi":"10.1093/jat/bkaf001","DOIUrl":"10.1093/jat/bkaf001","url":null,"abstract":"<p><p>In postmortem forensic investigation cases where the bladder is voided or dehydrated prior to autopsy, it is possible to wash the bladder with saline to collect the \"bladder wash\" and any residual urine for toxicological analysis. While not conventional, this study aims to determine the use of bladder washes as alternative specimens in postmortem forensic toxicology. Comprehensive drug and alcohol analysis was performed on blood, urine, vitreous humor, and bladder wash samples. Control studies consisted of matched bladder wash and urine samples for comparison. Authentic applicability studies were performed on bladder wash samples in cases where only blood or no urine samples were available. Bladder wash testing via the routine urine methodology was shown to have the appropriate sensitivity and specificity to serve as an alternative specimen. Specificity of the applicability studies was further improved when comparisons were corrected by evaluating individual analytes jointly with their related parent drug or metabolites. Individual and corrected sensitivity and specificity rates of above 99% were typically observed in both comparisons against urine and blood paired samples. Following drug analysis of 31 cases in which only a bladder wash was available, 57 detections from 23 different analytes were detected that otherwise would not have been obtained. This study demonstrates that standardized collection of the easily accessible bladder wash for postmortem toxicological analysis serves forensic toxicologists and pathologists with invaluable information where urine or other biological specimens are not available.</p>","PeriodicalId":14905,"journal":{"name":"Journal of analytical toxicology","volume":" ","pages":"180-190"},"PeriodicalIF":2.3,"publicationDate":"2025-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142970663","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Toxicological evaluation, postmortem case descriptions, and pharmacological activity of N,N-dimethylpentylone and related analogs.","authors":"Melissa F Fogarty, Sara E Walton, Michael T Truver, Grant C Glatfelter, Alex J Krotulski, Donna M Papsun, Michael Lamb, Chris W Chronister, Bruce A Goldberger, Donna Walther, Kristie Barba, Michael H Baumann, Barry K Logan","doi":"10.1093/jat/bkaf002","DOIUrl":"10.1093/jat/bkaf002","url":null,"abstract":"<p><p>Identification of N,N-dimethylpentylone (DMP) in counterfeit \"Ecstasy\" and \"Molly\" tablets poses risk to public health due to its adverse effects. Little information is available regarding the pharmacological activity or relevant blood or tissue concentrations of DMP, and even less is known about other structurally related beta-keto methylenedioxyamphetamine analogs on recreational drug markets, such as N-propyl butylone. Here, a novel toxicological assay utilizing liquid chromatography-tandem quadrupole mass spectrometry was developed and validated for the quantitation of DMP and five related synthetic cathinones [eutylone, pentylone, N-ethyl pentylone (NEP), N-propyl butylone, and N-cyclohexyl butylone], with chromatographic resolution from isomeric variants and quantitation performed by standard addition. A forensic series of 125 cases is presented for DMP and related analogs, along with pharmacological activity assessments using monoamine transporter and mouse behavioral assays. The blood concentration range for DMP in postmortem forensic cases was 3.3-4600 ng/mL (mean: 320 ± 570 ng/mL, median: 150 ng/mL), whereas pentylone, the primary N-desmethyl metabolite of DMP, was identified in 98% of cases with a concentration range 1.3-710 ng/mL (mean ± SD: 105 ± 120 ng/mL, median: 71 ng/mL). N-Propyl butylone, a newly identified synthetic cathinone, was quantitated in seven cases (mean ± SD: 82 ± 75 ng/mL, median: 50 ng/mL, range: 1.7-200 ng/mL). DMP displayed potent uptake inhibition at the dopamine transporter [half maximal inhibitory concentration (IC50) of 49 nM], with 100-fold weaker potency at the serotonin transporter (IC50 = 4990 nM). DMP was a locomotor stimulant in mice [medium effective dose (ED50) of 3.5 mg/kg] exhibiting potency relatively similar to eutylone, NEP, and pentylone. Our results show that DMP is a psychomotor stimulant associated with adverse clinical outcomes leading to death. Forensic laboratories must continue to update testing methods to capture emerging drugs, with specific emphasis on resolution and identification of isomeric species. Following the scheduling of DMP in early 2024, there could be an anticipated market shift toward a new unregulated synthetic stimulant to replace DMP.</p>","PeriodicalId":14905,"journal":{"name":"Journal of analytical toxicology","volume":" ","pages":"143-151"},"PeriodicalIF":2.3,"publicationDate":"2025-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11892558/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143046535","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Opioid hair concentrations using retrospective prescription data from a United States workplace testing population.","authors":"G Neil Stowe, Ryan B Paulsen, Michael I Schaffer","doi":"10.1093/jat/bkae101","DOIUrl":"10.1093/jat/bkae101","url":null,"abstract":"<p><p>Opioids are widely prescribed pain medications that have the potential for misuse and abuse. As part of a routine procedure, Psychemedics frequently encounters questions from clients/Medical Review Officers regarding opioid hair concentrations in relation to the amount of opioids taken as part of a prescription. In this article, we have analyzed a large number of real-world examples of opioid hair concentrations following self-reported consumption of an opioid prescription regimen. This dataset provides a reference point of opioid hair concentrations after an extensive aqueous wash that likely corresponds to consumption of an opioid prescription regimen. Practitioners in the field could use this reference to make decisions on the opioid concentration of a hair sample in relation to a client-provided prescription.</p>","PeriodicalId":14905,"journal":{"name":"Journal of analytical toxicology","volume":" ","pages":"201-207"},"PeriodicalIF":2.3,"publicationDate":"2025-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142921689","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Correction to: Drug detection in oral fluid and urine after single therapeutic doses of dexamphetamine, lisdexamphetamine, and methylphenidate in healthy volunteers.","authors":"","doi":"10.1093/jat/bkaf008","DOIUrl":"10.1093/jat/bkaf008","url":null,"abstract":"","PeriodicalId":14905,"journal":{"name":"Journal of analytical toxicology","volume":" ","pages":"e1"},"PeriodicalIF":2.3,"publicationDate":"2025-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11892549/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143425333","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Toxicological and Demographic Profiles of Phencyclidine (PCP)-Impaired Driving Cases in Houston: Updates from the 2019-2023 Data.","authors":"Dayong Lee, Salvador R Corral, Cassandra Duvall, Peter Stout","doi":"10.1093/jat/bkaf021","DOIUrl":"https://doi.org/10.1093/jat/bkaf021","url":null,"abstract":"<p><p>Phencyclidine (PCP) is a dissociative anesthetic harmful to road traffic safety as the drug may impair driving performance by inducing adverse effects such as sedation, ataxia, agitation, disorientation, and confusion. Houston Forensic Science Center (HFSC) previously reported toxicological and demographic characteristics of PCP-impaired driving cases in Houston from 2013 to 2018 and presently reports the 2019-2023 cases. The blood samples collected from suspect drivers were analyzed for alcohol and drugs and those positive for PCP at the reporting limit of 5 ng/mL were included in the study (n = 1,375). The drivers had the median (mean, range) PCP concentration of 45 (49, 5-170) ng/mL and were mostly males (77%) and black (89%) with the mean age of 40 years. More than half of the drivers (59%) were polydrug users with cannabinoids being the most frequently detected (39%), followed by cocaine/metabolites (15%) and ethanol (10%). Compared to our previous findings and other studies, the PCP concentration distributions and concurrent drug profiles of the drivers were remarkably consistent despite multiple changes in the drug market over the years; their demographics also remained comparable except for the mean age, which continued to increase. Continual surveillance of PCP-impaired driving cases is important to identify risk groups and aid in reducing this hazardous driving behavior, so prevalent and persistent in the city of Houston.</p>","PeriodicalId":14905,"journal":{"name":"Journal of analytical toxicology","volume":" ","pages":""},"PeriodicalIF":2.3,"publicationDate":"2025-03-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143567160","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"HIV Combination Drug Therapies: Development and Validation of an LC-MS/MS Method for Simultaneous Quantitation of Abacavir, Dolutegravir, and Lamivudine in Rat Matrices in Support of Toxicology Studies.","authors":"Melanie A Rehder Silinski, Jennifer A Gilliam, Julia Apoian, Brenda L Fletcher, Reshan A Fernando, Suramya Waidyanatha","doi":"10.1093/jat/bkaf016","DOIUrl":"https://doi.org/10.1093/jat/bkaf016","url":null,"abstract":"<p><p>Abacavir (ABC), Dolutegravir (DTG), and Lamivudine (3TC) are part of a fixed-dose combination medication for treatment of HIV. The three drugs offer different but complementary mechanisms of action by inhibiting reverse transcriptase and integrase, and ultimately inhibiting HIV replication. Due to lack of information regarding long-term safety following in utero exposure, we are evaluating potential toxicity to offspring following in utero exposure to this combination therapy in Hsd:Sprague Dawley®SD® (HSD) rats, including cardiovascular toxicity and neurotoxicity. Generating internal exposure data are integral to putting toxicological findings into context. The objective of this work was to develop and validate a method to simultaneously quantitate ABC, DTG, and 3TC in rat matrices following exposure to this combination. The method used protein precipitation of plasma, fetal, placental, brain, or heart homogenate followed by ultra-performance liquid chromatography-tandem mass spectrometry. In adult Sprague Dawley rat plasma, the method was linear (r≥0.99) over the range 10/15/5 to 10,000/15,000/5000 ng/mL for ABC/DTG/3TC and recovery was ≥92% for all three analytes at all concentration levels. The limits of detection were 2.22, 3.69, and 0.978 ng/mL for ABC, DTG, and 3TC, respectively. Intra- and inter-day precision was ≤8.7% relative standard deviation (RSD), and RE ≤±12.0% for standards prepared at 20/30/10, 400/600/200, and 5000/7500/2500 ng/mL. Matrix standards as high as 40/60/20 µg/mL could be diluted into the calibration range (RE≤±3.5% and RSD ≤2.4%). The method was evaluated for HSD rat maternal plasma and fetal, placental, brain, and heart homogenates (mean RE ≤±15.0% and RSD ≤8.6%). Analyte stability was demonstrated in extracted plasma for two days at different temperatures, and in various matrices stored at -80°C for at least 32 days (80-113% of Day 0 concentrations). These data demonstrate that this simple and efficient method is suitable for quantitation of ABC, DTG, and 3TC in rat matrices generated from toxicology studies. The method can easily be adapted to other biological matrices and species (e.g., human).</p>","PeriodicalId":14905,"journal":{"name":"Journal of analytical toxicology","volume":" ","pages":""},"PeriodicalIF":2.3,"publicationDate":"2025-02-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143556872","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}