Forensic Chemistry最新文献

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 : 2026-01-27 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

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 : 2026-01-14 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

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 : 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

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 : 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

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 : 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

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 : 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

Assessing the expanded capacity of modern μ-XRF SDD systems for forensic analysis through an interlaboratory study: Part I—Electrical tapes 通过实验室间研究评估用于法医分析的现代μ-XRF SDD系统的扩展容量：第一部分-电气磁带

IF 2.2 3区医学 Q2 CHEMISTRY, ANALYTICAL

Forensic Chemistry

Pub Date : 2025-12-18 DOI: 10.1016/j.forc.2025.100719

Lacey Leatherland , Zachary Andrews , Cedric Neumann , John Chester , Mirjam de Bruin-Hoegée , Troy Ernst , Kris Gates , Susan Gross , Anne Kisler-Rao , Arian van Asten , Tatiana Trejos

Recent modernization of micro-X-ray Fluorescence Spectrometry (μ-XRF) instrumentation has increased capabilities for elemental analysis in forensic casework. In this study, the analytical performance of several μ-XRF instrument configurations, each equipped with silicon drift detectors (SDDs), is assessed through an interlaboratory study (ILS) using two novel poly(vinyl chloride) (PVC) matrix-matched standards (de Bruin-Hoegée et al., 2023 [1]). Also, the informative value of μ-XRF in casework-like electrical tape samples is evaluated, and a quantitative metric known as spectral contrast angle ratio (SCAR) for spectral data interpretation is mathematically normalized. The ILS evaluates inter-instrumental and inter-examiner variability in comparing and interpreting spectral data. The ILS exercise consists of ten sets of electrical tapes from various ground truth sources (same roll, same package, different rolls), each with five sections per set. Data is collected across eight laboratories, with 11 instrumental configurations. Results from spectral overlay and SCAR pairwise comparisons (45 each) are compared between each laboratory and each set of instrumental parameters (495 comparison pairs, 15 replicates per sample). The results of this study reinforce the utility of μ-XRF in tape examinations and indicate strong inter-laboratory agreement, with low false-inclusion and exclusion rates (<2.4 % and < 4.6 %, respectively). The study demonstrates the benefits of comparing SCAR metrics across laboratories. The observed trends in detection capabilities across different instrumental configurations can help identify relevant parameters for consistent analysis and interpretation across different laboratories and future methodology implementation in forensic casework. Ultimately, standardized interpretation adds value to the tape evidence to further substantiate conclusions during investigative stages and in the courtroom.

最近现代化的微x射线荧光光谱（μ-XRF）仪器增加了法医案件中元素分析的能力。在本研究中，使用两种新型聚氯乙烯（PVC）基质匹配标准（de bruin - hoeg et al., 2023[1]），通过实验室间研究（ILS）评估了几种μ-XRF仪器配置的分析性能，每种配置都配备了硅漂移检测器（sdd）。此外，还评估了μ-XRF在案例样电工带样品中的信息价值，并对光谱数据解释的定量度量光谱对比角比（SCAR）进行了数学归一化。ILS在比较和解释光谱数据时评估仪器间和观测者间的可变性。盲测练习包括十套来自不同接地真相来源的电气胶带（同一卷，同一包，不同卷），每套有五个部分。数据在8个实验室收集，有11种仪器配置。光谱叠加和SCAR两两比较（各45对）的结果在每个实验室和每组仪器参数之间进行比较（495对比较，每个样品15个重复）。本研究的结果加强了μ-XRF在磁带检查中的实用性，并表明实验室间一致性强，假包含率和排除率低（分别为2.4%和4.6%）。该研究证明了跨实验室比较SCAR指标的好处。观察到的不同仪器配置的检测能力趋势可以帮助确定相关参数，以便在不同实验室之间进行一致的分析和解释，并在法医案件工作中实施未来的方法。最终，标准化的解释增加了磁带证据的价值，从而在调查阶段和法庭上进一步证实结论。

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引用次数: 0

Developing incremental isotope sampling methods for the dental enamel of human canines and molars 发展人类犬齿和磨牙牙釉质的增量同位素取样方法

IF 2.2 3区医学 Q2 CHEMISTRY, ANALYTICAL

Forensic Chemistry

Pub Date : 2025-12-18 DOI: 10.1016/j.forc.2025.100720

Jacob I. Griffith , Hannah F. James , Barbara Veselka , Rick J. Schulting , Christina Cheung , Lisette M. Kootker , Matija Črešnar , Tamara Leskovar , Hai-Yen Tran , Philippe Claeys , Hugues Gregoir , Christophe Snoeck

The isotope analysis of human dental enamel has become an essential tool in forensic and archaeological science for reconstructing childhood diet, mobility, and geographic provenance. Enamel forms during early life and does not remodel, permanently incorporating isotopic values such as δ¹³C, δ¹⁸O, and ⁸⁷Sr/⁸⁶Sr ingested at the time. The majority of studies rely on a singular bulk enamel sample from an individual to determine birthplace, but this approach overlooks isotope variation within the enamel. This study aims to enhance enamel isotope analysis by constructing and expanding incremental enamel sampling techniques to track childhood mobility and diet at a higher resolution.

The Plomp et al. (2020) methodology for third molars (M3) was replicated and applied to first molars (M1), with the addition of a fourth sampling increment near the enamel-root junction. A new standardised method for hand-drilled incremental sampling of canines was also developed, guided by thin sections of enamel growth patterns. While molars yielded overlapping increments due to complex growth patterns and wear, canines provided up to four distinct, minimally overlapping increments spanning 1.5–7 years of age.

These methods effectively capture gradual and abrupt shifts in mobility and diet in time-resolved order, which are not detectable in bulk samples. The results suggest that canines may offer improved chronological resolution compared to molars due to the latter's growth complexity and more substantial wear. This study demonstrates the potential of incremental enamel sampling for reconstructing individual life histories and aiding the identification of unknown individuals in forensic contexts.

人类牙釉质的同位素分析已经成为法医和考古科学中重建儿童饮食、活动和地理来源的重要工具。牙釉质在生命早期形成，不会重塑，永久地吸收了当时摄入的同位素值，如δ13C、δ18O和87Sr/86Sr。大多数研究依赖于个体的单一散装牙釉质样本来确定出生地，但这种方法忽略了牙釉质内部的同位素变化。本研究旨在通过构建和扩展珐琅质增量采样技术，以更高的分辨率跟踪儿童的活动和饮食，从而增强珐琅质同位素分析。Plomp等人（2020）对第三磨牙（M3）的方法被复制并应用于第一磨牙（M1），并在牙釉质-牙根交界处附近增加了第四个采样增量。在牙釉质生长模式的薄片指导下，还开发了一种新的标准化方法，用于手工钻孔的犬类增量采样。由于复杂的生长模式和磨损，磨牙产生了重叠的增量，而犬齿在1.5-7岁之间提供了多达四个不同的，最小重叠的增量。这些方法有效地捕获了在时间分辨顺序中逐渐和突然的移动和饮食变化，这在大量样品中是无法检测到的。结果表明，由于磨牙的生长复杂性和更大的磨损，犬科动物可能比磨牙提供更好的时间分辨率。本研究证明了牙釉质取样在重建个体生活史和帮助鉴定法医背景下未知个体方面的潜力。

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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 : 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

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 : 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