Forensic Chemistry最新文献

Rapid static headspace GC approach for screening of chloropicrin in environmental and urban samples 快速静态顶空气相色谱法筛选环境和城市样品中的氯霉素

IF 2.9 3区医学

Forensic Chemistry Pub Date : 2026-09-01 Epub Date: 2026-08-25 DOI: 10.1016/j.forc.2026.100773

Tomáš Rozsypal

{"title":"Rapid static headspace GC approach for screening of chloropicrin in environmental and urban samples","authors":"Tomáš Rozsypal","doi":"10.1016/j.forc.2026.100773","DOIUrl":"10.1016/j.forc.2026.100773","url":null,"abstract":"<div><div>Chloropicrin (trichloronitromethane) is a highly volatile toxic compound used as a fumigant and historically as a chemical warfare agent. Renewed interest in chloropicrin has emerged following reports and investigations of its possible use in recent armed conflicts. However, its rapid dissipation presents significant challenges for forensic investigations, where delayed sampling and storage may compromise successful identification. In this study, a static headspace gas chromatography–flame ionization detection (HS–GC–FID) method was developed and optimized for chloropicrin determination and subsequently applied to investigate its recovery, persistence and storage stability in representative matrices. Key parameters were systematically optimized, including extraction temperature, equilibration time, injected headspace volume, split ratio and inlet temperature. The optimized method provided satisfactory linearity, repeatability and matrix recoveries. The method was applied to contaminated concrete, sand, soil, water, wipe, bitumen, PVC and polystyrene samples. Apparent dissipation half-lives ranged from 0.2 to 2.3 h at room temperature and 1.1–16.4 h at 5 °C, confirming the rapid disappearance of chloropicrin from most surfaces and the strong influence of temperature on its persistence. Storage experiments demonstrated that sample preservation conditions substantially affected analytical outcomes. Frozen storage generally provided the highest retained recoveries, whereas room-temperature storage frequently resulted in significant analyte losses. Vial closure type also influenced chloropicrin preservation, with the investigated screw-cap vial system consistently outperforming the tested crimp-top configuration. The results demonstrate that reliable chloropicrin detection depends not only on analytical methodology but also on appropriate sampling and storage procedures. The presented data provide practical guidance for chemical incident response involving chloropicrin.</div></div>","PeriodicalId":324,"journal":{"name":"Forensic Chemistry","volume":"50 ","pages":"Article 100773"},"PeriodicalIF":2.9,"publicationDate":"2026-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148854394","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}

引用次数: 0

Preliminary Chemical Analysis of Latent Fingermarks Developed with Fire Extinguisher Dry Powder by Matrix-Assisted Laser Desorption/Ionization Mass Spectrometry Imaging 用基质辅助激光解吸/电离质谱成像技术初步分析灭火器干粉形成的手印

IF 2.2 3区医学

Forensic Chemistry Pub Date : 2026-05-01 Epub Date: 2026-01-27 DOI: 10.1016/j.forc.2026.100726

Deejay Suen-yui Mak , Ming-yip Fung , Zhong-Ping Yao

{"title":"Preliminary Chemical Analysis of Latent Fingermarks Developed with Fire Extinguisher Dry Powder by Matrix-Assisted Laser Desorption/Ionization Mass Spectrometry Imaging","authors":"Deejay Suen-yui Mak , Ming-yip Fung , Zhong-Ping Yao","doi":"10.1016/j.forc.2026.100726","DOIUrl":"10.1016/j.forc.2026.100726","url":null,"abstract":"<div><div>Latent fingermarks, which are frequently present on evidence items at crime scenes, are one of the most powerful types of physical evidence because of their uniqueness and their substantial value in biometric identification. Current fingermark development methods fail to detect all the invisible fingermarks, and it can be very time consuming and labour-intensive when processing large crime scenes and bulky evidence items with large surface areas. Here we report for the first time the application of matrix-assisted desorption/ionization mass spectrometry imaging (MALDI-MSI) for the chemical analysis of latent fingermarks developed with an <em>in situ</em> detection method that makes use of dry powder from a fire extinguisher. The spraying process of fire extinguisher dry powder allows latent fingermarks to be developed within seconds at crime scenes, while imaging of each developed fingermark allows simultaneous pattern visualization and chemical analysis for building a profile of the individual who left the fingermark. We demonstrate that the optimized method of matrix application can be used to reveal the complex molecular information of various endogenous compounds and exogenous compounds embedded in the powder-developed fingermarks at a micron-scale resolution. Operational use of the method is further supported by successful separation of overlapping powder-treated fingermarks without disturbing the fingermark patterns. Our method effectively combines the advantages of fire extinguisher dry powder as an <em>in-situ</em> fingermark development technique with MALDI-MSI which shows the significant potential for the powder to be integrated into the routine fingermark forensic analysis.</div></div>","PeriodicalId":324,"journal":{"name":"Forensic Chemistry","volume":"48 ","pages":"Article 100726"},"PeriodicalIF":2.2,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146102827","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}

引用次数: 0

Separation and quantification of novel synthetic regioisomeric fentanyls in clinical extracts by high pH reverse-phase LC-MS/MS 高pH反相LC-MS/MS分离和定量芬太尼临床提取物中新型合成区域异构体

IF 2.2 3区医学

Forensic Chemistry Pub Date : 2026-03-01 Epub Date: 2025-12-18 DOI: 10.1016/j.forc.2025.100721

Benjamin S. Barrett , Jennifer K. Field , Erika Sitch , William H. Campbell , Melvin R. Euerby , Oliver B. Sutcliffe

{"title":"Separation and quantification of novel synthetic regioisomeric fentanyls in clinical extracts by high pH reverse-phase LC-MS/MS","authors":"Benjamin S. Barrett , Jennifer K. Field , Erika Sitch , William H. Campbell , Melvin R. Euerby , Oliver B. Sutcliffe","doi":"10.1016/j.forc.2025.100721","DOIUrl":"10.1016/j.forc.2025.100721","url":null,"abstract":"<div><div>This study compares three different chromatographic methods used for the separation of regioisomeric fluorofentanyl, as described in previous literature, through application to clinical whole blood extracts. A high pH, RP-UHPLC-MS/MS method was selected and a series of opioids (<em>n</em> = 23), including regioisomeric series of fluorofentanyl, despropionylfluorofentanyl, and fluoroisobutyrylfentanyl (<em>n</em> = 13), fentanyl and other fentanyl analogues (<em>n</em> = 8), heroin and xylazine, were successfully validated against UKAS LAB51 and SWGTOX guidelines using this method. The results of the validation demonstrated R<sup>2</sup> greater than 0.99 for all analytes except heroin (<em>n</em> = 22), accuracy ranging from 96.8 % to 110.1 % and precision between 0.8 % to 13.2 % as percentage coefficient of variation across replicate injections (<em>n</em> = 9) of three different quality control levels for all analytes except heroin (n = 22). Limits of detection ranged from 0.016 ng/mL to 0.24 ng/mL and limits of quantification ranged from 0.049 ng/mL to 0.729 ng/mL. Clinical whole blood extracts were screened by high-resolution mass spectrometry and triaged for further identification and quantification of regioisomeric compounds where an unknown regioisomeric form of fluorofentanyl was found. Across all sample extracts <em>para</em>-fluorofentanyl was successfully identified, alongside potential interferences including other drugs of abuse (cocaine, methamphetamine, gabapentin) and cutting agents (procaine, lidocaine), and quantified within the range of 0.44 ng/mL to 31.16 ng/mL, with fentanyl, <em>para</em>-despropionylfluorofentanyl, and 4-ANPP detected and quantified in all samples with <em>para</em>-fluorofentanyl.</div></div>","PeriodicalId":324,"journal":{"name":"Forensic Chemistry","volume":"47 ","pages":"Article 100721"},"PeriodicalIF":2.2,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145836474","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}

引用次数: 0

Analysis of saxitoxin and analogues by reverse-phase liquid chromatography coupled to mass spectrometry after derivatisation with ethyl chloroformate 氯甲酸乙酯衍生后反相液相色谱-质谱联用分析蛤蚌毒素及其类似物

IF 2.2 3区医学

Forensic Chemistry Pub Date : 2026-03-01 Epub Date: 2026-01-14 DOI: 10.1016/j.forc.2026.100725

Karina Vignati, George Kaklamanos, Adriaan Marais, Daniel Noort, Prabhakar Sripadi, Yue Wang, Nathan W. McGill

{"title":"Analysis of saxitoxin and analogues by reverse-phase liquid chromatography coupled to mass spectrometry after derivatisation with ethyl chloroformate","authors":"Karina Vignati, George Kaklamanos, Adriaan Marais, Daniel Noort, Prabhakar Sripadi, Yue Wang, Nathan W. McGill","doi":"10.1016/j.forc.2026.100725","DOIUrl":"10.1016/j.forc.2026.100725","url":null,"abstract":"<div><div>Verification of saxitoxin (STX), a Schedule 1 chemical under the Chemical Weapons Convention, requires highly selective analytical methods for diverse sample types. In this study, STX was derivatised with ethyl chloroformate to form less polar derivatives without compromising the structural differences that differentiate it from non-scheduled congeners. Following optimisation of the derivatisation conditions, the method was applied to STX-spiked samples relevant to chemical weapons testing scenarios including authentic sample analysis and chemical forensics. The protocol enabled the rapid and selective identification of STX at 40 ppb in water and beverages in the presence of non-scheduled congeners including neosaxitoxin, decarbamoyl saxitoxin, and decarbamoyl neosaxitoxin by reverse-phase liquid chromatography mass spectrometry (LC-MS). Additionally, samples from the Organisation for the Prohibition of Chemical Weapons First Trial Biotoxin Proficiency Test were derivatised and analysed, facilitating the identification of a blank sample and two samples spiked with STX at the ppb level. Finally, the protocol was applied to contaminated oyster homogenate to demonstrate its utility in a food matrix. The protocol was found to complement existing methods for the analysis of STX in a chemical weapons verification context and rapidly produces analytical data for verification of STX in several types of samples. The ability to distinguish STX from non-scheduled congeners by reverse-phase LC-MS, which is a standard technique in most chemical weapon residue testing laboratories, is a further benefit of this work.</div></div>","PeriodicalId":324,"journal":{"name":"Forensic Chemistry","volume":"47 ","pages":"Article 100725"},"PeriodicalIF":2.2,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146022595","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}

引用次数: 0

Discrimination of synthetic cannabinoids using 80 MHz benchtop NMR: MDA-19 and its analogues 用80 MHz台式核磁共振鉴别合成大麻素：MDA-19及其类似物

IF 2.2 3区医学

Forensic Chemistry Pub Date : 2026-03-01 Epub Date: 2025-12-12 DOI: 10.1016/j.forc.2025.100718

Sojeon Moon , Soyoung Park , Hyemin Kim , Jihwan Park , Seonghye Kim , Sujin Lee , Suhkmann Kim

{"title":"Discrimination of synthetic cannabinoids using 80 MHz benchtop NMR: MDA-19 and its analogues","authors":"Sojeon Moon , Soyoung Park , Hyemin Kim , Jihwan Park , Seonghye Kim , Sujin Lee , Suhkmann Kim","doi":"10.1016/j.forc.2025.100718","DOIUrl":"10.1016/j.forc.2025.100718","url":null,"abstract":"<div><div>The widespread emergence of New Psychoactive Substances (NPS) continues to challenge forensic laboratories, particularly when structurally related synthetic cannabinoids must be distinguished early in the analytical process. MDA-19, originally developed as a selective CB<sub>2</sub> receptor agonist, is now frequently encountered in illicit drug markets along with its closely related analogues such as 5C-MDA-19 and 5F-MDA-19. Their high structural similarity often leads to overlapping spectral patterns and complicates rapid field-forward screening.</div><div>In this study, we demonstrate that an 80 MHz benchtop NMR spectrometer—a compact and readily accessible analytical platform—can reliably differentiate MDA-19 and its analogues. Distinctive <sup>1</sup>H NMR features were identified for each compound, and two-dimensional <sup>1</sup>H–<sup>13</sup>C HSQC experiments provided diagnostic cross-peaks that resolved key structural ambiguities. The combined spectral signatures indicated that the three analogues can be reproducibly distinguished even under mixture conditions.</div><div>These findings highlight the operational utility of benchtop NMR for the rapid characterization of synthetic cannabinoids. In particular, HSQC offers high diagnostic value for discriminating structurally similar analogues, underscoring its potential integration into early-stage triage, seized-drug assessment, and on-site forensic workflows.</div></div>","PeriodicalId":324,"journal":{"name":"Forensic Chemistry","volume":"47 ","pages":"Article 100718"},"PeriodicalIF":2.2,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145787469","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}

引用次数: 0

From on-site color change to forensic evidence: Smartphone-operated tristimulus evaluation of detection tubes for chemical warfare agent vapors 从现场颜色变化到法医证据：智能手机操作的化学战剂蒸汽检测管的三刺激评估

IF 2.2 3区医学

Forensic Chemistry Pub Date : 2026-03-01 Epub Date: 2025-11-27 DOI: 10.1016/j.forc.2025.100714

Tomas Rozsypal , Victor Bocos-Bintintan

{"title":"From on-site color change to forensic evidence: Smartphone-operated tristimulus evaluation of detection tubes for chemical warfare agent vapors","authors":"Tomas Rozsypal , Victor Bocos-Bintintan","doi":"10.1016/j.forc.2025.100714","DOIUrl":"10.1016/j.forc.2025.100714","url":null,"abstract":"<div><div>Rapid, objective, and defensible detection of chemical warfare agents .CWAs) at incident scenes remains a critical challenge in forensic chemistry. Detector tubes, widely used by military and emergency services, are low-cost and simple but traditionally provide only subjective yes/no results. Here, we demonstrate the first field-deployable approach that upgrades these tubes into semi-quantitative forensic tools by coupling them with an inexpensive portable tristimulus colorimeter that can be operated either directly on-device or via a free Android application.</div><div>Using tubes for sarin (GB), hydrogen cyanide (AC), and sulfur mustard (HD), color responses were evaluated in CIE-L*a*b* space. Analytical parameters—including repeatability at fixed spots, intra−/interday precision, calibration models, stabilization times, and colorimetric detection thresholds (CDTs)—were systematically characterized. Instrumental colorimetry reduced CDTs by approximately one order of magnitude (5–20×) compared to conventional naked-eye inspection, providing faster, more reproducible, and quantifiable results. Calibration was linear for AC and HD and followed a power-law model for GB, with uncertainties ≤15 % except for heterogeneous AC layers (≤40 %).</div><div>This workflow converts subjective visual inspection into objective, archivable digital records suitable for forensic documentation. Compared to advanced field instruments such as ion mobility spectrometers, it delivers actionable semi-quantitative data at a fraction of the cost and logistical burden. While the method is inherently limited by the heterogeneity of indicator layers and possible matrix effects, these factors do not outweigh its forensic advantages, particularly its enhanced sensitivity, reproducibility, and trace-level applicability for both military and civilian chemical incident response.</div></div>","PeriodicalId":324,"journal":{"name":"Forensic Chemistry","volume":"47 ","pages":"Article 100714"},"PeriodicalIF":2.2,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145617276","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}

引用次数: 0

Controlled smoking of methamphetamine in a car and initial remediation by ventilation: Analysing air, surfaces and fabrics 控制在车内吸食甲基苯丙胺及通过通风进行初步补救：分析空气、表面和织物

IF 2.2 3区医学

Forensic Chemistry Pub Date : 2026-03-01 Epub Date: 2025-12-25 DOI: 10.1016/j.forc.2025.100723

Gemma L. Kerry , Kirstin E. Ross , Jackie Wright , G. Stewart Walker

{"title":"Controlled smoking of methamphetamine in a car and initial remediation by ventilation: Analysing air, surfaces and fabrics","authors":"Gemma L. Kerry , Kirstin E. Ross , Jackie Wright , G. Stewart Walker","doi":"10.1016/j.forc.2025.100723","DOIUrl":"10.1016/j.forc.2025.100723","url":null,"abstract":"<div><div>Methamphetamine is smoked in vehicles leading to contamination and possible thirdhand exposure risks. This study was performed to determine the extent and distribution of methamphetamine after controlled smoking of the drug within a car. After three controlled smoking events over three weeks, the car windows were opened for ventilation for eight weeks. Air sampling, surface wipe sampling, and fabric sampling were performed after smoking and ventilation. All samples were extracted using a modified version of the National Institute for Occupational Safety and Health (NIOSH) 9111 method for methamphetamine by liquid chromatography-mass spectrometry (LC-MS). Methamphetamine was detected in air in the passenger compartment and rear storage areas using XAD-2 resin sorbent tubes ranging from 0.19 to 0.96 μg/m<sup>3</sup>. Concentrations ranged from 0.02 to 41.2 μg/100 cm<sup>2</sup> for car fabric surfaces and 0.17 to 3.66 μg/sample for the plastic air vents. Cotton, faux leather, neoprene, and polyester fabrics were placed on the seats and sampled after the smoking events and venting periods. Cotton ranged from 1.68 to 32.3 μg/sample, faux leather from 1.27 to 16.6 μg/sample, neoprene from 0.46 to 15.5 μg/sample and polyester from 0.41 to 2.36 μg/sample. Methamphetamine detected from air, surfaces, and fabrics in a car after controlled smoking of a total of 0.6 g of methamphetamine hydrochloride indicate widespread contamination of materials in the car and potential for thirdhand exposure. Methamphetamine was detected at lower concentrations after eight weeks ventilation from air, on surfaces, and on fabrics, indicating the potential for some extent of remediation.</div></div>","PeriodicalId":324,"journal":{"name":"Forensic Chemistry","volume":"47 ","pages":"Article 100723"},"PeriodicalIF":2.2,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145972963","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}

引用次数: 0

GC–MS and GC–MS/MS analysis of regioisomeric N-dimethoxybenzyl derivatives of 2-, 3-, and 4-methoxyphenylpiperazines 2-、3-和4-甲氧基苯基哌嗪的n -二甲氧基苯基区域异构体衍生物的GC-MS和GC-MS /MS分析

IF 2.2 3区医学

Forensic Chemistry Pub Date : 2026-03-01 Epub Date: 2025-12-31 DOI: 10.1016/j.forc.2025.100722

C. Randall Clark , Younis Abiedalla

{"title":"GC–MS and GC–MS/MS analysis of regioisomeric N-dimethoxybenzyl derivatives of 2-, 3-, and 4-methoxyphenylpiperazines","authors":"C. Randall Clark , Younis Abiedalla","doi":"10.1016/j.forc.2025.100722","DOIUrl":"10.1016/j.forc.2025.100722","url":null,"abstract":"<div><div>A series of <em>N</em>,<em>N</em>-disubstituted piperazines were synthesized containing the structural elements of methoxyphenylpiperazines and dimethoxybenzylpiperazines. These potential designer-like drug analogs were prepared based on common designer trends and their regioisomeric differentiation was based on GC–MS and GC–MS/MS studies. Capillary GC results revealed that the isomers eluted according to the position of aromatic ring substitution and/or the degree of substituent crowding on the aromatic ring. Numerous EI mass spectral ions occur via processes initiated by one of the two nitrogen atoms of the piperazine ring. This project focused on the determination of fragment ion structures and postulation of mechanisms for their formation. These studies were enabled by synthesizing stable isotope analogs, homologs, and monosubstituted piperazine model compounds. Based on the appropriate mass shifts for these fragments, a pattern of fragment structure and origin was established. All the eighteen isomers show an intense molecular radical cation at <em>m/z</em> 342 and a cationic fragment at <em>m/z</em> 191 from the loss of the substituted benzyl radical. Several low intensity ions in the higher mass range represent loss of methyl and methoxy radicals and a fragment radical cation resulting from ethene loss from the piperazine ring of the molecular radical cation. The labeled compounds allowed for the determination of which methyl and methoxy groups were involved in fragment formation. The fragments at <em>m/z</em> 151 (for all isomers) and <em>m/z</em> 136 (for the 2,3-dimethoxybenzyl substituted isomers) were determined to represent a mixture of isobaric ions occurring via decomposition from each of the piperazine substituents.</div></div>","PeriodicalId":324,"journal":{"name":"Forensic Chemistry","volume":"47 ","pages":"Article 100722"},"PeriodicalIF":2.2,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145920732","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}

引用次数: 0

Simultaneous analysis of opioid drugs used for pain in whole blood using liquid chromatography/time-of-flight mass spectrometry coupled with dried blood spots and solid-phase dispersive extraction 用液相色谱/飞行时间质谱联用干血斑和固相分散萃取法同时分析全血中用于止痛的阿片类药物

IF 2.2 3区医学

Forensic Chemistry Pub Date : 2026-03-01 Epub Date: 2025-12-09 DOI: 10.1016/j.forc.2025.100717

Koichi Saito, Rika Nishiyama, Rie Ito

{"title":"Simultaneous analysis of opioid drugs used for pain in whole blood using liquid chromatography/time-of-flight mass spectrometry coupled with dried blood spots and solid-phase dispersive extraction","authors":"Koichi Saito, Rika Nishiyama, Rie Ito","doi":"10.1016/j.forc.2025.100717","DOIUrl":"10.1016/j.forc.2025.100717","url":null,"abstract":"<div><div>This study targeted 11 opioid analgesics with a high potential for dependence and abuse—morphine, fentanyl, oxycodone, methadone, pethidine, codeine, tramadol, pentazocine, buprenorphine, naloxone, and <em>O</em>-desmethyltramadol—to develop a rapid, simple, and sensitive screening method for whole blood analysis. A pretreatment procedure was established that combines dried blood spot (DBS) extraction with solid-phase dispersive extraction (SPDE) cleanup using Captiva ND <sup><em>Lipids</em></sup> to remove phospholipids effectively. Analysis was performed by liquid chromatography coupled with time-of-flight mass spectrometry (LC/TOF-MS). The combined DBS–SPDE approach improved the precision of the recovery tests, and peaks likely originating from phospholipids observed with DBS extraction alone disappeared, indicating efficient phospholipid removal. The limits of detection and quantification for the 11 opioids were 0.02–0.05 ng/mL and 0.05–0.1 ng/mL, respectively. Validation results showed good trueness for most opioids (83.6–115.7 %), although morphine, buprenorphine, and naloxone exhibited lower values (24.2–49.0 %). Precision was satisfactory, with repeatability below 15 % and intermediate precision below 20 % for most analytes, except for morphine and buprenorphine, which showed slightly higher variability. These findings demonstrate that the proposed LC/TOF-MS method achieves sufficient sensitivity and reproducibility for screening purposes. The method offers a practical tool for identifying opioids and monitoring therapeutic drug levels in forensic and clinical applications.</div></div>","PeriodicalId":324,"journal":{"name":"Forensic Chemistry","volume":"47 ","pages":"Article 100717"},"PeriodicalIF":2.2,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145733755","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}

引用次数: 0

Turn-on fluorescence detection of trace methamphetamine for on-site forensic analysis with analyte recovery 开启荧光检测痕量甲基苯丙胺的现场法医分析与分析物回收

IF 2.2 3区医学

Forensic Chemistry Pub Date : 2026-03-01 Epub Date: 2025-12-27 DOI: 10.1016/j.forc.2025.100724

Seiya Awata , Futoshi Kikuchi , Toru Oba

{"title":"Turn-on fluorescence detection of trace methamphetamine for on-site forensic analysis with analyte recovery","authors":"Seiya Awata , Futoshi Kikuchi , Toru Oba","doi":"10.1016/j.forc.2025.100724","DOIUrl":"10.1016/j.forc.2025.100724","url":null,"abstract":"<div><div>The widespread abuse of methamphetamine (MA) highlights the need to develop rapid, simple, and cost-effective on-site screening methods to support forensic analysis. This study developed a turn-on fluorescence method for the naked-eye detection of MA based on host–guest interactions with cucurbit[7]uril (CB[7]). A fluorescent indicator forms a pre-complex with CB[7], and MA selectively displaces the indicator, enhancing fluorescence. To improve the field applicability, the method was adapted to a spray test that mimics luminol testing. The assay enabled naked-eye detection of as little as 50 ng of MA hydrochloride, with minimal interference from common substances, and demonstrated robustness against variations in ionic strength (up to ∼1 mM), temperature (10–40 °C), and long-term reagent stability (≥250 days). Importantly, MA was recovered with 94–110 % efficiency, enabling confirmatory analysis via mass spectrometry. These findings highlight the potential of the supramolecular fluorescence assay as a practical and low-cost strategy for rapid on-site screening of trace MA while preserving the original analyte for downstream confirmatory analysis.</div></div>","PeriodicalId":324,"journal":{"name":"Forensic Chemistry","volume":"47 ","pages":"Article 100724"},"PeriodicalIF":2.2,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145880356","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}

引用次数: 0