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 Q2 CHEMISTRY, ANALYTICAL

Forensic Chemistry

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

Tomáš Rozsypal

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.

氯丁（三氯硝基甲烷）是一种高度挥发性的有毒化合物，用作熏蒸剂，历史上曾用作化学战剂。在对氯丁可能在最近的武装冲突中使用进行报告和调查之后，人们重新对氯丁产生了兴趣。然而，它的快速消散对法医调查提出了重大挑战，其中延迟采样和存储可能会影响成功的鉴定。本研究建立并优化了静态顶空气相色谱-火焰离子化检测（HS-GC-FID）测定氯苦苷的方法，并对其在代表性基质中的回收率、持久性和储存稳定性进行了研究。对萃取温度、平衡时间、注入顶空容积、分流比和进口温度等关键参数进行了系统优化。优化后的方法具有良好的线性、重复性和回收率。该方法适用于污染的混凝土、沙子、土壤、水、擦拭、沥青、PVC和聚苯乙烯样品。在室温下的表观耗散半衰期为0.2 ~ 2.3 h，在5℃下为1.1 ~ 16.4 h，证实了氯丁在大多数表面上的快速消失以及温度对其持久性的强烈影响。储存实验表明，样品保存条件对分析结果有很大影响。冷冻储存通常提供最高的保留回收率，而室温储存经常导致显著的分析物损失。小瓶封闭类型也影响氯霉素保存，所研究的螺旋盖小瓶系统始终优于所测试的卷曲顶部配置。结果表明，可靠的氯霉素检测不仅取决于分析方法，而且取决于适当的取样和储存程序。所提出的数据为涉及氯仿的化学事件响应提供了实际指导。

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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 Q2 CHEMISTRY, ANALYTICAL

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

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 in situ 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 in-situ fingermark development technique with MALDI-MSI which shows the significant potential for the powder to be integrated into the routine fingermark forensic analysis.

由于其独特性和在生物识别中的巨大价值，隐性手印是最有力的物证之一，经常出现在犯罪现场的证物上。目前的手印开发方法无法检测到所有不可见的手印，而且在处理大型犯罪现场和体积庞大、表面积大的物证时，费时费力。本文首次报道了基质辅助解吸/电离质谱成像（MALDI-MSI）在原位检测方法（利用灭火器干粉）开发的潜在手印化学分析中的应用。灭火器干粉的喷洒过程可以在几秒钟内在犯罪现场形成潜在的手印，而每个形成的手印的成像可以同时实现模式可视化和化学分析，从而建立留下手印的个人的轮廓。我们证明，优化的基质应用方法可以在微米级分辨率上揭示嵌入在粉末形成的手印中的各种内源化合物和外源化合物的复杂分子信息。通过成功分离重叠的粉末处理手印而不干扰手印图案，进一步支持了该方法的操作使用。我们的方法有效地结合了灭火器干粉作为原位手印显示技术与MALDI-MSI的优点，显示了将干粉集成到常规手印法医分析中的巨大潜力。

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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 Q2 CHEMISTRY, ANALYTICAL

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

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 (n = 23), including regioisomeric series of fluorofentanyl, despropionylfluorofentanyl, and fluoroisobutyrylfentanyl (n = 13), fentanyl and other fentanyl analogues (n = 8), heroin and xylazine, were successfully validated against UKAS LAB51 and SWGTOX guidelines using this method. The results of the validation demonstrated R² greater than 0.99 for all analytes except heroin (n = 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 (n = 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 para-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, para-despropionylfluorofentanyl, and 4-ANPP detected and quantified in all samples with para-fluorofentanyl.

本研究比较了三种不同的色谱方法用于分离区域异构体氟芬太尼，如以往文献所述，通过应用于临床全血提取物。采用高pH、RP-UHPLC-MS/MS方法，对一系列阿片类药物（n = 23），包括氟芬太尼、地丙基氟芬太尼、氟异丁基芬太尼（n = 13）、芬太尼及其他芬太尼类似物（n = 8）、海洛因和噻嗪，根据UKAS LAB51和SWGTOX指南成功进行了验证。验证结果表明，除海洛因（n = 22）外，除海洛因（n = 22）外，3种不同质量控制水平的重复注射（n = 9）的准确度在96.8% ~ 110.1%之间，精密度在0.8% ~ 13.2%之间。检测限为0.016 ~ 0.24 ng/mL，定量限为0.049 ~ 0.729 ng/mL。临床全血提取物通过高分辨率质谱法进行筛选，并进行分类，以便在发现未知区域异构体形式的氟芬太尼时进一步鉴定和定量区域异构体化合物。在所有样品提取物中，对氟芬太尼都被成功地鉴定出来，同时还有潜在的干扰因素，包括其他滥用药物（可卡因、甲基苯丙胺、加巴喷丁）和切割剂（普鲁卡因、利多卡因），并在0.44 ng/mL至31.16 ng/mL的范围内进行了定量，所有样品中对氟芬太尼、对地丙基氟芬太尼和4-ANPP都被检测出来，并在对氟芬太尼中进行了定量。

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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 Q2 CHEMISTRY, ANALYTICAL

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

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.

作为《化学武器公约》的附表1化学品，对蛤蚌毒素的核查需要对不同类型的样品采用高度选择性的分析方法。在这项研究中，STX与氯甲酸乙酯衍生，形成极性较小的衍生物，而不影响其与非计划同源物的结构差异。在优化衍生化条件后，该方法被应用于与化学武器测试场景相关的stx加标样品，包括真实样品分析和化学法医。该方案能够通过反相液相色谱-质谱（LC-MS）快速和选择性地鉴定水和饮料中40 ppb的STX，其中存在非计划同源物，包括新石蜡毒素，decarbamoyl石蜡毒素和decarbamoyl新石蜡毒素。此外，对来自禁止化学武器组织第一次生物毒素熟练度试验的样本进行了衍生和分析，有助于鉴定一个空白样本和两个含有STX的样品，其含量达到ppb水平。最后，将该方案应用于受污染的牡蛎匀浆，以证明其在食品基质中的实用性。发现该议定书补充了化学武器核查中分析STX的现有方法，并迅速产生了用于核查几种样品中的STX的分析数据。通过反相LC-MS区分STX和非计划同源物的能力是这项工作的另一个好处，这是大多数化学武器残留测试实验室的标准技术。

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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 Q2 CHEMISTRY, ANALYTICAL

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

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 CB₂ 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.

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 ¹H NMR features were identified for each compound, and two-dimensional ¹H–¹³C 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.

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.

新精神活性物质（NPS）的广泛出现继续挑战法医实验室，特别是当结构相关的合成大麻素必须在分析过程的早期区分。MDA-19最初是作为一种选择性CB2受体激动剂开发的，现在在非法药物市场上经常遇到与其密切相关的类似物，如5C-MDA-19和5F-MDA-19。它们的高结构相似性往往导致重叠的光谱模式和复杂的快速场前筛选。在这项研究中，我们证明了80 MHz台式核磁共振光谱仪-一个紧凑且易于访问的分析平台-可以可靠地区分MDA-19及其类似物。每个化合物都有独特的1H NMR特征，二维1H - 13c HSQC实验提供了诊断交叉峰，解决了关键的结构歧异。综合光谱特征表明，即使在混合条件下，这三种类似物也可以重复地区分。这些发现突出了台式核磁共振快速表征合成大麻素的操作效用。特别是，HSQC在鉴别结构相似的类似物方面提供了很高的诊断价值，强调了它在早期分诊、缉获药物评估和现场法医工作流程中的潜在集成。

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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 Q2 CHEMISTRY, ANALYTICAL

Forensic Chemistry

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

Tomas Rozsypal , Victor Bocos-Bintintan

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.

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 %).

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.

快速、客观、可防御的化学战剂探测。在事故现场的CWAs仍然是法医化学的一个关键挑战。探测管广泛用于军事和应急服务，成本低且简单，但传统上只能提供主观的是/否结果。在这里，我们展示了第一种可现场部署的方法，将这些管升级为半定量法医工具，通过将它们与廉价的便携式三刺激色度计相结合，可以直接在设备上操作，也可以通过免费的Android应用程序操作。使用沙林（GB）、氰化氢（AC）和芥子气（HD）的色谱管，在CIE-L*a*b*空间中评价颜色反应。分析参数-包括定点重复性，日内/日间精度，校准模型，稳定时间和比色检测阈值(CDTs) -系统表征。与传统的裸眼检测相比，仪器比色法将CDTs降低了大约一个数量级（5 - 20倍），提供了更快、更可重复性和可量化的结果。AC和HD的校准是线性的，GB的校准遵循幂律模型，除异质AC层（≤40%）外，不确定性≤15%。该工作流程将主观的视觉检查转换为客观的、可归档的数字记录，适用于法医文件。与先进的现场仪器（如离子迁移谱仪）相比，它可以以很小的成本和后勤负担提供可操作的半定量数据。虽然该方法受到指示层的异质性和可能的矩阵效应的固有限制，但这些因素并没有超过其法医优势，特别是其增强的灵敏度、可重复性和对军用和民用化学事件响应的痕量水平适用性。

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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 Q2 CHEMISTRY, ANALYTICAL

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

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/m³. Concentrations ranged from 0.02 to 41.2 μg/100 cm² 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.

在车辆内吸食甲基苯丙胺，导致污染和可能的三手接触风险。这项研究是为了确定在汽车内控制吸烟后甲基苯丙胺的程度和分布。在三周内进行三次控制吸烟事件后，打开车窗通风八周。吸烟和通风后进行空气取样、表面擦拭取样和织物取样。所有样品均采用改进版的美国国家职业安全与卫生研究所（NIOSH） 9111甲基苯丙胺液相色谱-质谱（LC-MS）提取方法。采用XAD-2型树脂吸附管对客舱和后储物区空气中的甲基苯丙胺进行检测，检测范围为0.19 ~ 0.96 μg/m3。汽车织物表面的浓度范围为0.02 ~ 41.2 μg/100 cm2，塑料通风口的浓度范围为0.17 ~ 3.66 μg/样品。在吸烟事件和排气期后，将棉、人造皮革、氯丁橡胶和聚酯织物放在座位上并取样。棉为1.68 ~ 32.3 μg/样，人造革为1.27 ~ 16.6 μg/样，氯丁橡胶为0.46 ~ 15.5 μg/样，涤纶为0.41 ~ 2.36 μg/样。在控制吸烟后，从车内的空气、表面和织物中检测出总共0.6克盐酸甲基苯丙胺，表明车内材料受到广泛污染，可能存在三手接触。在空气通风八周后，在表面和织物上检测到甲基苯丙胺的浓度较低，表明有一定程度的修复潜力。

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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 Q2 CHEMISTRY, ANALYTICAL

Forensic Chemistry

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

C. Randall Clark , Younis Abiedalla

A series of N,N-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 m/z 342 and a cationic fragment at m/z 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 m/z 151 (for all isomers) and m/z 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.

合成了一系列含有甲氧基苯基哌嗪和二甲氧基苯基哌嗪结构元素的N，N-二取代哌嗪。这些潜在的设计器样药物类似物是基于共同的设计器趋势制备的，其区域异构体分化基于GC-MS和GC-MS /MS研究。毛细管气相色谱结果表明，同分异构体的洗脱依据是芳香环取代位置和取代基在芳香环上的密集程度。许多EI质谱离子通过哌嗪环的两个氮原子之一引发的过程发生。本项目的重点是片段离子结构的确定和它们形成机制的假设。这些研究是通过合成稳定同位素类似物、同源物和单取代哌嗪模型化合物来实现的。根据这些碎片的适当质量位移，建立了碎片结构和起源模式。所有18个同分异构体在m/z 342处都有一个强烈的分子自由基阳离子，在m/z 191处由于取代的苄基自由基的丢失而有一个阳离子片段。在高质量范围内的几个低强度离子代表甲基和甲氧基自由基的损失，以及由分子自由基阳离子的哌嗪环上的乙烯损失引起的碎片自由基阳离子。标记的化合物允许确定哪些甲基和甲氧基参与片段的形成。在m/z 151（所有异构体）和m/z 136（2,3-二甲氧基苄基取代异构体）的片段被确定为通过分解从每个哌嗪取代基产生的等压离子的混合物。

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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 Q2 CHEMISTRY, ANALYTICAL

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

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 O-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 ^Lipids 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.

本研究针对吗啡、芬太尼、羟考酮、美沙酮、哌替啶、可待因、曲马多、戊唑嗪、丁丙诺啡、纳洛酮、o -去甲基曲马多等11种依赖性和滥用可能性高的阿片类镇痛药，建立一种快速、简便、灵敏的全血筛查方法。建立了一种将干血斑（DBS）萃取与固相分散萃取（SPDE）清洗相结合的预处理工艺，使用Captiva ND Lipids有效地去除磷脂。采用液相色谱-飞行时间质谱法（LC/TOF-MS）进行分析。DBS - spde联合方法提高了回收率测试的精度，DBS单独提取观察到的磷脂可能产生的峰消失，表明有效的磷脂去除。11种阿片类药物的检出限和定量限分别为0.02 ~ 0.05 ng/mL和0.05 ~ 0.1 ng/mL。验证结果显示，大多数阿片类药物的正确率为83.6 ~ 115.7%，吗啡、丁丙诺啡和纳洛酮的正确率较低（24.2 ~ 49.0%）。精密度令人满意，大多数分析物的重复性低于15%，中间精密度低于20%，但吗啡和丁丙诺啡的变异性略高。这些结果表明，LC/TOF-MS方法具有足够的灵敏度和可重复性。该方法为鉴定阿片类药物和监测法医和临床应用中的治疗药物水平提供了实用工具。

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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 Q2 CHEMISTRY, ANALYTICAL

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

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.

甲基苯丙胺（MA）的广泛滥用突出表明需要开发快速、简单和具有成本效益的现场筛选方法，以支持法医分析。本研究建立了一种基于与葫芦b[7] （CB[7]）的主客体相互作用的MA裸眼检测的开启荧光方法。荧光指示剂与CB[7]形成预络合物，MA选择性地取代指示剂，增强荧光。为了提高现场适用性，将该方法应用于模拟鲁米诺测试的喷雾测试中。该方法可以裸眼检测到50ng的盐酸MA，受普通物质的干扰最小，并且对离子强度（高达~ 1mm）、温度（10-40°C）和长期试剂稳定性（≥250天）的变化具有鲁棒性。重要的是，MA回收率为94 - 110%，可以通过质谱进行验证分析。这些发现突出了超分子荧光分析作为一种实用的低成本策略的潜力，可以快速现场筛选痕量MA，同时保留原始分析物用于下游验证分析。

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引用次数: 0