Forensic Chemistry最新文献

Development of a semi-preparative LC method for the purification of synthetic cannabinoids impregnated in herbal products for chemical characterization by NMR and HRMS 建立一种半制备液相色谱法，用于纯化浸渍在草药产品中的合成大麻素，并通过NMR和HRMS进行化学表征

IF 2.6 3区医学

Forensic Chemistry Pub Date : 2025-06-10 DOI: 10.1016/j.forc.2025.100678

Karen Rafaela Gonçalves de Araújo , Gabriela de Paula Meirelles , Daniel Pecoraro Demarque , Fabiane Dorr , Luiz Ferreira Neves Júnior , Alexandre Learth Soares , Camila Delanesi Guedes , José Luiz da Costa , Mauricio Yonamine

{"title":"Development of a semi-preparative LC method for the purification of synthetic cannabinoids impregnated in herbal products for chemical characterization by NMR and HRMS","authors":"Karen Rafaela Gonçalves de Araújo , Gabriela de Paula Meirelles , Daniel Pecoraro Demarque , Fabiane Dorr , Luiz Ferreira Neves Júnior , Alexandre Learth Soares , Camila Delanesi Guedes , José Luiz da Costa , Mauricio Yonamine","doi":"10.1016/j.forc.2025.100678","DOIUrl":"10.1016/j.forc.2025.100678","url":null,"abstract":"<div><div>Synthetic cannabinoids (SCs) now encompass over 360 compounds under international control. Identifying these substances is a significant challenge for law enforcement, as they are new drugs found in herbal fragments, and reference standards are not available for traditional chemical analysis. To address this, substances can be identified using type A analytical techniques, according to the Scientific Working Group for the Analysis of Seized Drugs which are those with the highest level of selectivity and provide structural information, such as nuclear magnetic resonance and mass spectrometry. However, these methods require compound purification for proper characterization. This study aimed to develop a purification method for SCs in herbal fragments to enable chemical analysis. Seized samples were first analyzed using gas chromatography-electron ionization-mass spectrometry (GC-EI-MS). Then, a semi-preparative liquid chromatography (LC) method was applied, successfully isolating SCs and allowing their structural determination through NMR and high-resolution mass spectroscopy. In the first sample, MDMB-CHMINACA was identified as the sole SC. In the second sample, GC-EI-MS analysis revealed a mass spectrum that did not match any library entry. After purification, the substance was identified as ADB-INACA. In the third sample, the method facilitated the separation and structural determination of four SCs (MDMB-INACA, ADB-BUTINACA, MDMB-4en-PINACA, and 5F-ADB) in a mixture from an herbal sample. In conclusion, the method developed for purification using semi-preparative LC for subsequent chemical characterization proved to be effective for the structural determination of new SCs present in herbal drugs seized by the police.</div></div>","PeriodicalId":324,"journal":{"name":"Forensic Chemistry","volume":"45 ","pages":"Article 100678"},"PeriodicalIF":2.6,"publicationDate":"2025-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144263554","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

A multi-modal spectroscopic approach to forensic discrimination of liquid cosmetic complexion products 一种多模态光谱方法用于液体化妆品的法医鉴别

IF 2.6 3区医学

Forensic Chemistry Pub Date : 2025-06-06 DOI: 10.1016/j.forc.2025.100677

Jesse McEwan , Katy A. Bruce , Kari Pitts , Georgina Sauzier

{"title":"A multi-modal spectroscopic approach to forensic discrimination of liquid cosmetic complexion products","authors":"Jesse McEwan , Katy A. Bruce , Kari Pitts , Georgina Sauzier","doi":"10.1016/j.forc.2025.100677","DOIUrl":"10.1016/j.forc.2025.100677","url":null,"abstract":"<div><div>Foundations and other complexion products such as concealers or beauty balm creams account for a significant proportion of the global cosmetic market. In addition to being widely used across a range of demographics, these products are inherently transferable through contact and have a variety of distinctive formulations, making them potentially valuable as associative evidence. Despite this, the analysis of complexion products for forensic purposes is a relatively under-researched area, with studies to date largely focussed exclusively on foundation products often analysed using a single technique. In this study, 35 liquid complexion products representing 19 international retailers available within Australia were analysed using ATR-FTIR spectroscopy. Initially indistinguishable samples were then analysed using Raman spectroscopy and X-ray diffraction, which have not previously been applied in the open literature for forensic cosmetic analysis, to enhance discrimination. Chemometric pattern recognition based on infrared data resulted in a discrimination accuracy of 98 % between individual products and classification accuracy of 72 % using a blind validation set. Raman spectroscopy and X-ray diffraction each offered enhanced discrimination of similar products primarily based on mineral content, although similar shades of the same product remain challenging. Analysis of eight duplicate samples purchased from the UK retail market revealed no significant compositional differences between batches from global retailers, which has yet to be explicitly investigated in existing studies. This market survey highlights the chemical variability of complexion products that may be exploited for evidential purposes using a multi-modal analytical workflow.</div></div>","PeriodicalId":324,"journal":{"name":"Forensic Chemistry","volume":"45 ","pages":"Article 100677"},"PeriodicalIF":2.6,"publicationDate":"2025-06-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144263553","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 automotive lubricating grease residue: A forensic investigation using ATR-FTIR spectroscopic and chemometric interpretation 汽车润滑油脂残留物的分析：ATR-FTIR光谱和化学计量学解释的法医调查

IF 2.6 3区医学

Forensic Chemistry Pub Date : 2025-05-29 DOI: 10.1016/j.forc.2025.100670

Dimple Bhatia, Chongtham Nimi, Deepak Kumar, Arti Yadav, Rajinder Singh

{"title":"Analysis of automotive lubricating grease residue: A forensic investigation using ATR-FTIR spectroscopic and chemometric interpretation","authors":"Dimple Bhatia, Chongtham Nimi, Deepak Kumar, Arti Yadav, Rajinder Singh","doi":"10.1016/j.forc.2025.100670","DOIUrl":"10.1016/j.forc.2025.100670","url":null,"abstract":"<div><div>Automotive lubricating greases are widely utilized in automobiles, making them frequently encountered trace evidence in incidents involving a vehicle's collision with another vehicle, person, animal, or stationary object. Due to their high transferability, lubricating grease can act as valuable corroborative evidence during crime scene investigations. They can assist in establishing a link between the vehicle and the individual (victim or accused) to the crime scene, while also confirming contact between the vehicle and the victim. In this study, 21 brands of automotive lubricating grease samples were analyzed for their identification and differentiation, employing a rapid and non-destructive ATR-FTIR spectroscopic technique combined with chemometrics. ATR-FTIR spectra of all samples were visually examined and categorized into six groups based on their similarities and differences. After visual examination, the training dataset was subjected to chemometric analysis using PCA and SVM tools. PCA was employed to explore trends within the dataset, while SVM classified samples, achieving 97.62 % training accuracy and 88.09 % external validation accuracy. To ensure an unbiased validation of the SVM model, the training and validation datasets were comprised of a distinct set of spectra. A blind test validated the SVM model, resulting in 100 % prediction accuracy. Additionally, a study was performed to evaluate how substrate type, storage conditions, and storage duration could affect the linking of the substrate grease samples to their source. The findings revealed that the above-mentioned factors, particularly sunlight exposure and the washing of the substrate grease samples, significantly influence the SVM prediction accuracy.</div></div>","PeriodicalId":324,"journal":{"name":"Forensic Chemistry","volume":"45 ","pages":"Article 100670"},"PeriodicalIF":2.6,"publicationDate":"2025-05-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144169950","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

Correlation of compositional change with visualization enhancement results and morphology evolution of blood based on thermal performance analysis 基于热性能分析的血液成分变化与可视化增强结果及形态演变的相关性研究

IF 2.6 3区医学

Forensic Chemistry Pub Date : 2025-05-26 DOI: 10.1016/j.forc.2025.100669

Junyi Di , Jing Jin , Zirui Lu , Xinyu Yan , Peibin Wang , Jinzhuan Zhang , Chaoyi Shi

{"title":"Correlation of compositional change with visualization enhancement results and morphology evolution of blood based on thermal performance analysis","authors":"Junyi Di , Jing Jin , Zirui Lu , Xinyu Yan , Peibin Wang , Jinzhuan Zhang , Chaoyi Shi","doi":"10.1016/j.forc.2025.100669","DOIUrl":"10.1016/j.forc.2025.100669","url":null,"abstract":"<div><div>The morphology evolution and compositional change of blood during heating are crucial for understanding the results of visualization enhancement when using chemical reagents. Given the complexity of blood composition, human and two other mammalian blood samples were initially centrifuged and prepared as dried whole blood, dried erythrocytes, and dried plasma for further TG-IR analysis. The results indicated that the decomposition process of blood could be divided into four distinct stages: 35-190 °C, 190-430 °C, 430-610 °C, and 610-800 °C. In the second stage, lipids and proteins underwent thermal decomposition, resulting in an approximately 50 % mass loss of blood with the release of NH<sub>3</sub> and CO<sub>2</sub>, and obvious bulges presented with a black metallic appearance due to the rapid release of gases. The bloodstains could be visualized by the luminol test after heating at 310 °C for 5 min. Also, a positive reaction could be obtained by using tetramethylbenzidine (TMB) after heating at 400 °C for 5 min. In the third stage, the mass loss was further reduced by approximately 40 %. The streaks or block-like fractures appeared on the surface, with the metallic luster largely disappearing. Negative visualization results were obtained from bloodstains after heating at 480 °C for 5 min, suggesting that the hemoglobin was completely decomposed. The thermal decomposition process was gradually decreased when heating above 610 °C and completed around 880 °C, with minimal fibrous residues left. The compositional changes of blood during heating were correlated with morphology evolution and visualization enhancement, providing the evidence for blood detection in fire scenes.</div></div>","PeriodicalId":324,"journal":{"name":"Forensic Chemistry","volume":"45 ","pages":"Article 100669"},"PeriodicalIF":2.6,"publicationDate":"2025-05-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144185910","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

Assessment of adsorption interference from carbonaceous materials in post-explosion residue analysis of fuel–oxidizer mixtures by ion chromatography 离子色谱法评价燃料-氧化剂混合物爆炸后残留物分析中碳质物质的吸附干扰

IF 2.6 3区医学

Forensic Chemistry Pub Date : 2025-05-22 DOI: 10.1016/j.forc.2025.100671

Lúcio Paulo Lima Logrado

{"title":"Assessment of adsorption interference from carbonaceous materials in post-explosion residue analysis of fuel–oxidizer mixtures by ion chromatography","authors":"Lúcio Paulo Lima Logrado","doi":"10.1016/j.forc.2025.100671","DOIUrl":"10.1016/j.forc.2025.100671","url":null,"abstract":"<div><div>This study investigated the influence of carbonaceous materials on the extraction and analysis of post-explosion residues by ion chromatography (IC). Three adsorptive materials—activated carbon, carbonized paper residue, and vegetal charcoal—were evaluated for their capacity to retain inorganic ions typically found in combustion/explosion residues of flash powder, black powder, and explosive emulsions. The targeted ions included Cl<sup>−</sup>, NO₂<sup>−</sup>, OCN<sup>−</sup>, ClO₃<sup>−</sup>, NO₃<sup>−</sup>, SO₄<sup>2−</sup>, S₂O₃<sup>2−</sup>, SCN<sup>−</sup>, ClO₄<sup>−</sup>, K<sup>+</sup>, NH₄<sup>+</sup>, and Na<sup>+</sup>. The results showed significant ion-specific retention effects, particularly for oxidizing anions, which varied depending on the type and amount of adsorbent. Additional experiments comparing room temperature and heated (90 °C) aqueous extractions demonstrated that heating does not provide a consistent solution to the problem of ion adsorption. These findings underscore the risk of false negatives or underestimation of analytes caused by the presence of carbon-rich debris, commonly found in post-explosion samples. The study highlights the importance of considering adsorptive interference when selecting sample portions for analysis, prioritizing areas with minimal carbonaceous content. These findings contribute to improving the reliability of IC and other aqueous extraction-based methods used in the forensic analysis of explosive residues.</div></div>","PeriodicalId":324,"journal":{"name":"Forensic Chemistry","volume":"44 ","pages":"Article 100671"},"PeriodicalIF":2.6,"publicationDate":"2025-05-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144146866","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 as a valuable tool for analysing cannabinoid-containing gummies and identifying the synthetic process used for their production 气相色谱-质谱是分析含大麻素软糖和鉴定其生产过程的有价值的工具

IF 2.6 3区医学

Forensic Chemistry Pub Date : 2025-05-21 DOI: 10.1016/j.forc.2025.100672

Arianna Bini , Elisa Roda , Stefano Protti , Luca Morini , Antonella Profumo , Marco Cavallo , Adolfo Gregori , Carlo Alessandro Locatelli , Daniele Merli

{"title":"GC–MS as a valuable tool for analysing cannabinoid-containing gummies and identifying the synthetic process used for their production","authors":"Arianna Bini , Elisa Roda , Stefano Protti , Luca Morini , Antonella Profumo , Marco Cavallo , Adolfo Gregori , Carlo Alessandro Locatelli , Daniele Merli","doi":"10.1016/j.forc.2025.100672","DOIUrl":"10.1016/j.forc.2025.100672","url":null,"abstract":"<div><div>Due to the growing commercial availability of cannabinoids as active principles for recreational use, the use of preparations including among the others extracts and edible products (e.g., gummy sweets) is gaining popularity when compared to smoking, the more classical method of cannabinoid consumption. In this context, along with the widely known cannabidiol (CBD) and Δ<sup>9</sup>-tetrahydrocannabinol (Δ<sup>9</sup>-THC), hexahydrocannabinol (HHC) and Δ<sup>8</sup>-tetrahydrocannabinol (Δ<sup>8</sup>-THC) have recently been openly sold in a range of products worldwide, having been neglected by some regulatory authorities.</div><div>When dealing with complex matrices such as edibles, the commonly available methods for the identification and quantification of natural and semi-synthetic cannabinoids – GC–MS and LC-MS – must be implemented. In this work, we describe a GC–MS protocol for the analysis of the different cannabinoids present in seized gummy sweets after liquid extraction of the active ingredients. The protocol has been optimized and validated (according to the current guidelines) by using spiked cannabinoid-free commercially available gummies. The procedure has been exploited for the identification and quantification of the cannabinoids (both natural and semisynthetic) present in six different types of seized recreational gummies and allowed us to hypothesize the origin of the cannabinoid -natural or synthetic- and in this last case also the synthetic strategies used to obtain them. Noteworthily, besides the cannabinoids already described in literature, our approach also pointed out the presence of a hexahydrocannabinol analogue (hexahydrocannabinonol, HHC-C9) as well as <em>cis</em>-9,10-octadecanoamide (oleamide), a modulator of CB1 cannabinoid receptor that exhibits a cannabinoid-like action.</div></div>","PeriodicalId":324,"journal":{"name":"Forensic Chemistry","volume":"44 ","pages":"Article 100672"},"PeriodicalIF":2.6,"publicationDate":"2025-05-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144125185","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

Elemental and isotopic profiling of potassium perchlorate salts for forensic explosives investigations 法医炸药调查用高氯酸钾的元素和同位素分析

IF 2.6 3区医学

Forensic Chemistry Pub Date : 2025-05-18 DOI: 10.1016/j.forc.2025.100666

I.M. van Damme , F.Y. Linzey , G.M.H. Brust , K. Haßler , C.D. van Dijk , A.E.D.M. van der Heijden , K.D.B. Bezemer , E. de Rijke , A.W.C. Hulsbergen , A.C. van Asten

{"title":"Elemental and isotopic profiling of potassium perchlorate salts for forensic explosives investigations","authors":"I.M. van Damme , F.Y. Linzey , G.M.H. Brust , K. Haßler , C.D. van Dijk , A.E.D.M. van der Heijden , K.D.B. Bezemer , E. de Rijke , A.W.C. Hulsbergen , A.C. van Asten","doi":"10.1016/j.forc.2025.100666","DOIUrl":"10.1016/j.forc.2025.100666","url":null,"abstract":"<div><div>This study explores the feasibility of using isotopic and elemental signatures for the source attribution of potassium perchlorate (KClO<sub>4</sub>) salts, which can play a significant role in forensic explosives investigations. A total of 41 different reference KClO<sub>4</sub> batches were analysed using isotope ratio mass spectrometry and inductively coupled plasma – mass spectrometry. Rubidium was the only elemental impurity detected consistently across all reference batches. Combined with the oxygen isotopic composition, these features provide a discriminating power of 94 %. A score-based likelihood ratio (LR) system was developed also including concentrations of sodium, magnesium, chromium, and iron, which were detected in 69–98 % of the reference samples and showed significant variation between sources. The LR system employs Manhattan distance and kernel density estimation to model (dis)similarity across source comparisons. Five-fold cross validation results suggest the LR system effectively distinguishes between same-source and different-source pairs (C<sub>llr</sub> = 0.184) and can be used to report LR values of up to 74 (moderate support). Infrequently detected trace elements and chlorate concentrations allow for a more comprehensive interpretation of chemical profile analyses and should also be considered to uphold forensic integrity. A series of tests have established a reliable method for the reduction of KClO₄ to KCl for subsequent chlorine isotope ratio – mass spectrometry (<em>δ</em><sup>37</sup>Cl -IRMS) measurements, which could provide additional discriminating power. Further research is required to develop a scalable process that yields sufficient material for <em>δ</em><sup>37</sup>Cl-IRMS and to ensure that the sample preparation process yields reproducible <em>δ</em><sup>37</sup>Cl values.</div></div>","PeriodicalId":324,"journal":{"name":"Forensic Chemistry","volume":"44 ","pages":"Article 100666"},"PeriodicalIF":2.6,"publicationDate":"2025-05-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144106847","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

Real-time monitoring and verification of scheduled-I chemicals in vapor phase combining chemical detector and SPME-GC 结合化学探测器和SPME-GC对气相中指定i类化学物质进行实时监测和验证

IF 2.6 3区医学

Forensic Chemistry Pub Date : 2025-05-17 DOI: 10.1016/j.forc.2025.100667

Madhav Varshney, Shiv Prakash Sharma, Abhay Narayan Yadav, Manorama Vimal, Rajkumar, Manisha Sathe, Vinod Kumar

{"title":"Real-time monitoring and verification of scheduled-I chemicals in vapor phase combining chemical detector and SPME-GC","authors":"Madhav Varshney, Shiv Prakash Sharma, Abhay Narayan Yadav, Manorama Vimal, Rajkumar, Manisha Sathe, Vinod Kumar","doi":"10.1016/j.forc.2025.100667","DOIUrl":"10.1016/j.forc.2025.100667","url":null,"abstract":"<div><div>We designed a vapor generator and interference mixing test setup that is reliable and stable to generate low-level standard vapors of CWAs with real-time monitoring and verification by combining a chemical detector, i.e., Flame Photometric Detector AP4C, and a gas chromatography with flame photometric detector (GC-FPD) combining with solid phase microextraction (SPME). Nerve agents (GA, GB, GD, and GF) and blister agent (HD) vapors were generated by the gas generation system and studied at a concentration of 0.05 mg m<sup>−3</sup> and 1.0 mg m<sup>−3</sup>, respectively. The long-term vapor stability up to 6 h was monitored (<em>n</em> = 60), ranging from 0.041 to 0.048 mg m<sup>−3</sup> (CV, 1.5–2.7) and 1.193 mg m<sup>−3</sup> (CV, 1.13) for nerve and blister agents, respectively. Results were obtained at 0 %, 35 %, and 75 % RH values for all selected analytes and compared statistically and found significant. For SPME analysis at the optimized parameter, 1 min sampling time was enough to analyse the vapor concentration. The test setup is capable of mixing vehicle exhaust to mimic field conditions. Additionally, the assessment of Analytical Greenness Metric for Sample Preparation (AGREEprep) and Blue Applicability Grade Index (BAGI) metric tools highlights the eco-friendly approach of this method.</div></div>","PeriodicalId":324,"journal":{"name":"Forensic Chemistry","volume":"44 ","pages":"Article 100667"},"PeriodicalIF":2.6,"publicationDate":"2025-05-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144089052","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

New perspectives on THCA decarboxylation and accurate GC–MS quantitation of Total THC in Cannabis using analyte protectants 使用分析物保护剂对大麻中THCA脱羧和总THC的GC-MS准确定量研究的新进展

IF 2.6 3区医学

Forensic Chemistry Pub Date : 2025-05-17 DOI: 10.1016/j.forc.2025.100668

Jerome Mulloor, Walter B. Wilson, Lane C. Sander

{"title":"New perspectives on THCA decarboxylation and accurate GC–MS quantitation of Total THC in Cannabis using analyte protectants","authors":"Jerome Mulloor, Walter B. Wilson, Lane C. Sander","doi":"10.1016/j.forc.2025.100668","DOIUrl":"10.1016/j.forc.2025.100668","url":null,"abstract":"<div><div>Forensic and commercial laboratories rely on well-characterized analytical methods to accurately determine total tetrahydrocannabinol (total THC), which is the sum of decarboxylated tetrahydrocannabinolic acid (THCA) and delta-9-tetrahydrocannabinol (Δ<sup>9</sup>-THC) in <em>Cannabis sativa</em> samples. The Agriculture Improvement Act of 2018 restricts the level of total THC allowed in <em>Cannabis</em> for classification as hemp for commercial purposes. Gas chromatography with mass spectrometry detection (GC–MS) is frequently employed for <em>Cannabis</em> measurements due to its simplicity and speed of analysis. However, several issues complicate the determination of total THC by GC–MS, which are well-documented but unresolved. In the current study, the origins of potential GC–MS method biases are investigated, and novel approaches are presented to mitigate interferences. The behavior of THCA and Δ<sup>9</sup>-THC during GC–MS analyses was studied extensively using test solutions containing their isotopically labeled analogs. A plant matrix effect was identified that significantly increased THCA and Δ<sup>9</sup>-THC responses for <em>Cannabis</em> extracts compared with calibrant solutions. A mechanism is proposed based on the interaction of THCA and Δ<sup>9</sup>-THC with silanols present on heated inlet surfaces. The use of active site blocking agents, known as analyte protectants, reduced these interactions and achieved suitable conditions for quantitation of total THC by GC–MS. When <em>Cannabis</em> plant extracts and calibrants were processed under the recommended conditions, the results were comparable to liquid chromatography with photodiode array (LC-PDA) analysis. The experimental findings ultimately provide evidence to explain the behavior of cannabinoids in the GC–MS system and offer new options for improving the accuracy of total THC measurements.</div></div>","PeriodicalId":324,"journal":{"name":"Forensic Chemistry","volume":"44 ","pages":"Article 100668"},"PeriodicalIF":2.6,"publicationDate":"2025-05-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144106848","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

Revealing novel ionic species and key forensic insights: comparative analysis of non-extracted seized tablets vs. corresponding extracts by DART-HRMS 揭示新的离子种类和关键的法医见解：用DART-HRMS对未提取的缉获片剂和相应的提取物进行比较分析

IF 2.6 3区医学

Forensic Chemistry Pub Date : 2025-05-09 DOI: 10.1016/j.forc.2025.100665

Alexandre Narcelli Pestana de Aguiar , Diego Rissi Carvalhosa , Francisco Radler de Aquino Neto , Gabriela Vanini

{"title":"Revealing novel ionic species and key forensic insights: comparative analysis of non-extracted seized tablets vs. corresponding extracts by DART-HRMS","authors":"Alexandre Narcelli Pestana de Aguiar , Diego Rissi Carvalhosa , Francisco Radler de Aquino Neto , Gabriela Vanini","doi":"10.1016/j.forc.2025.100665","DOIUrl":"10.1016/j.forc.2025.100665","url":null,"abstract":"<div><div>The modern drug market encompasses a wide variety of chemical structures present simultaneously in individual matrices, making it nearly impossible to efficiently extract all substances using a single, standardized extraction procedure. Nevertheless, many of these substances hold forensic value and can assist forensic authorities in their investigative efforts. Direct Analysis in Real Time (DART) is an ion source that has gained prominence due to its speed and ability to eliminate the need for sample extraction. However, unextracted solid analysis through DART can produce unknown ionic species, such as clusters and adducts, complicating result interpretation. This study qualitatively analyzed six seized tablets in both solid form and as extracts using direct analysis in real time high-resolution mass spectrometry (DART-HRMS), employing a non-targeted approach to highlight key differences. The comparative analysis revealed that several synthetic impurities, adulterants, and contaminants—such as fentanyl analogues, N-MEC, N-formyl-MDA, and N-formyl-MDMA—were exclusively detected through the direct analysis of unextracted tablets, with some present solely in a cluster form. Additionally, previously unreported ionic species were identified. Direct analysis of unextracted matrices provided valuable information that was lost during sample extraction, while the phenomenon of cluster formation proved beneficial by enhancing the detection of analytes. The identified synthetic impurities elucidated the synthetic route used in the manufacture of the seized tablets, whereas specific adulterants and contaminants shed light on drug manufacturing practices. The identification of these impurities, adulterants, and contaminants exclusively through the direct analysis of unextracted solids demonstrates DART-HRMS's ability to provide quicker and more comprehensive chemical profiling of seized drugs.</div></div>","PeriodicalId":324,"journal":{"name":"Forensic Chemistry","volume":"44 ","pages":"Article 100665"},"PeriodicalIF":2.6,"publicationDate":"2025-05-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143943536","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