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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 Q2 CHEMISTRY, ANALYTICAL 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
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 Δ9-tetrahydrocannabinol (Δ9-THC), hexahydrocannabinol (HHC) and Δ8-tetrahydrocannabinol (Δ8-THC) have recently been openly sold in a range of products worldwide, having been neglected by some regulatory authorities.
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 cis-9,10-octadecanoamide (oleamide), a modulator of CB1 cannabinoid receptor that exhibits a cannabinoid-like action.
由于大麻素作为娱乐用途的活性原理在商业上的可用性越来越高,与吸烟相比,包括其他提取物和可食用产品(例如,软糖)在内的制剂的使用越来越受欢迎,吸烟是大麻素消费的更经典的方法。在这种情况下,随着众所周知的大麻二酚(CBD)和Δ9-tetrahydrocannabinol (Δ9-THC),六氢大麻酚(HHC)和Δ8-tetrahydrocannabinol (Δ8-THC)最近在全球范围内公开销售一系列产品,被一些监管机构忽视。当处理复杂的基质,如可食用的,通常用于鉴定和定量天然和半合成大麻素的方法- GC-MS和LC-MS -必须实施。在这项工作中,我们描述了一种GC-MS协议,用于分析在液体提取活性成分后缉获的软糖中存在的不同大麻素。通过使用不含大麻素的商业口香糖,该方案已被优化和验证(根据现行指南)。该程序已被用于识别和定量大麻素(天然和半合成)存在于六种不同类型的缉获娱乐口香糖中,并允许我们假设大麻素的起源-天然或合成-以及在最后一种情况下用于获得它们的合成策略。值得注意的是,除了文献中已经描述的大麻素外,我们的方法还指出了六氢大麻酚类似物(hexahydrocannabinonol, HHC-C9)以及顺式9,10-十八烷酰胺(oleamide)的存在,这是CB1大麻素受体的调节剂,具有类似大麻素的作用。
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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 Q2 CHEMISTRY, ANALYTICAL 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
This study explores the feasibility of using isotopic and elemental signatures for the source attribution of potassium perchlorate (KClO4) salts, which can play a significant role in forensic explosives investigations. A total of 41 different reference KClO4 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 (Cllr = 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 (δ37Cl -IRMS) measurements, which could provide additional discriminating power. Further research is required to develop a scalable process that yields sufficient material for δ37Cl-IRMS and to ensure that the sample preparation process yields reproducible δ37Cl values.
本研究探讨了利用同位素和元素特征分析高氯酸钾(KClO4)盐来源归属的可行性,这将在法医爆炸物调查中发挥重要作用。采用同位素比质谱法和电感耦合等离子体质谱法对41批不同的KClO4参比进行了分析。铷是唯一在所有参考批次中一致检测到的元素杂质。结合氧同位素组成,这些特征提供了94%的鉴别能力。建立了基于分数的似然比(LR)系统,包括钠、镁、铬和铁的浓度,在69 - 98%的参考样品中检测到,并且在来源之间显示出显着差异。LR系统采用曼哈顿距离和核密度估计来模拟跨源比较的(非)相似性。五重交叉验证结果表明,LR系统可以有效区分同源和不同源对(Cllr = 0.184),并可用于报告LR值高达74(中等支持)。很少检测到的微量元素和氯酸盐浓度允许对化学剖面分析进行更全面的解释,也应考虑维护法医的完整性。一系列试验建立了一种可靠的方法,将KClO₄还原为KCl,用于随后的氯同位素比-质谱(δ37Cl - irms)测量,可以提供额外的判别能力。进一步的研究需要开发一种可扩展的工艺,以产生足够的δ37Cl- irms材料,并确保样品制备过程产生可重复的δ37Cl值。
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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 Q2 CHEMISTRY, ANALYTICAL 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
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−3 and 1.0 mg m−3, respectively. The long-term vapor stability up to 6 h was monitored (n = 60), ranging from 0.041 to 0.048 mg m−3 (CV, 1.5–2.7) and 1.193 mg m−3 (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.
结合化学检测器AP4C火焰光度检测器和气相色谱-火焰光度检测器(GC-FPD)结合固相微萃取(SPME)技术,设计了一套可靠稳定的蒸汽发生器和干扰混合测试装置,可生成低水平标准CWAs蒸汽,并进行实时监测和验证。神经毒剂(GA、GB、GD和GF)和起泡剂(HD)蒸汽由气体发生系统产生,分别在0.05 mg m−3和1.0 mg m−3的浓度下进行研究。监测了长达6小时的长期蒸汽稳定性(n = 60),神经剂和水疱剂分别为0.041至0.048 mg m - 3 (CV, 1.5-2.7)和1.193 mg m - 3 (CV, 1.13)。所有选定的分析物在0%、35%和75% RH值下获得结果,并进行统计学比较,发现显著性。对于优化参数下的SPME分析,1 min的采样时间足以分析蒸汽浓度。该测试装置能够混合车辆尾气以模拟现场条件。此外,对样品制备的分析绿色度量(AGREEprep)和蓝色适用性等级指数(BAGI)度量工具的评估强调了该方法的环保方法。
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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 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2025-05-17 DOI: 10.1016/j.forc.2025.100668
Jerome Mulloor, Walter B. Wilson, Lane C. Sander
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 (Δ9-THC) in Cannabis sativa samples. The Agriculture Improvement Act of 2018 restricts the level of total THC allowed in Cannabis for classification as hemp for commercial purposes. Gas chromatography with mass spectrometry detection (GC–MS) is frequently employed for Cannabis 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 Δ9-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 Δ9-THC responses for Cannabis extracts compared with calibrant solutions. A mechanism is proposed based on the interaction of THCA and Δ9-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 Cannabis 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.
法医和商业实验室依靠特性良好的分析方法来准确测定大麻样品中的总四氢大麻酚(THC),即脱羧四氢大麻酚酸(THCA)和德尔塔-9-四氢大麻酚(Δ9-THC)的总和。2018年的《农业改进法》限制了大麻中允许的四氢大麻酚总量,将其归类为商业用途的大麻。气相色谱-质谱检测(GC-MS)由于其简单和分析速度快,经常用于大麻测量。然而,一些问题使气相色谱-质谱法测定总四氢大麻酚复杂化,这些问题有充分的文献记录,但尚未解决。在当前的研究中,研究了潜在的GC-MS方法偏差的来源,并提出了新的方法来减轻干扰。使用含有THCA和Δ9-THC同位素标记类似物的测试溶液,广泛研究了THCA和Δ9-THC在GC-MS分析中的行为。与校准溶液相比,植物基质效应显著提高了大麻提取物的THCA和Δ9-THC响应。提出了一种基于THCA和Δ9-THC与加热进口表面上存在的硅烷醇相互作用的机制。活性位点阻断剂(被称为分析物保护剂)的使用减少了这些相互作用,并为GC-MS定量总四氢大麻酚提供了合适的条件。当大麻植物提取物和校准剂在推荐的条件下处理时,结果与光电二极管阵列(LC-PDA)液相色谱分析相当。实验结果最终为解释大麻素在GC-MS系统中的行为提供了证据,并为提高总四氢大麻酚测量的准确性提供了新的选择。
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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 Q2 CHEMISTRY, ANALYTICAL 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
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.
现代药品市场包含同时存在于单个基质中的多种化学结构,使得使用单一的标准化提取程序有效提取所有物质几乎是不可能的。然而,其中许多物质具有法医价值,可以协助法医当局进行调查工作。直接实时分析(DART)是一种离子源,由于其速度和消除样品提取需求的能力而获得突出地位。然而,通过DART进行未提取的固体分析可能会产生未知的离子种类,如簇和加合物,使结果解释复杂化。本研究采用实时高分辨率质谱(DART-HRMS)直接分析方法,对6种被查获的片剂进行了定性分析,包括固体形式和提取物,采用非靶向方法来突出关键差异。对比分析显示,几种合成杂质、掺假物和污染物,如芬太尼类似物、N-MEC、n -甲酰基mda和n -甲酰基mdma,通过对未提取片剂的直接分析可以完全检测到,其中一些仅以簇状形式存在。此外,还发现了以前未报道的离子种类。直接分析未提取的矩阵提供了在样品提取过程中丢失的有价值的信息,而簇形成现象通过增强分析物的检测被证明是有益的。鉴定出的合成杂质阐明了制造被查获药片所用的合成路线,而特定的掺杂物和污染物则阐明了药物生产实践。通过直接分析未提取的固体来识别这些杂质、掺假物和污染物,证明了DART-HRMS能够提供更快、更全面的缉获药物化学分析。
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引用次数: 0
Analysis of Flubromazepam positional isomers for forensic differentiation 氟溴西泮位置异构体法医鉴别分析
IF 2.6 3区 医学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2025-05-01 DOI: 10.1016/j.forc.2025.100664
Evelyn S. Ligon , Ariel N. Parker , Ashley Braxton , Stefan France , B. McKay Allred
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引用次数: 0
Electrodeposition of redox materials with potential for enhanced visualisation of latent finger-marks on brass substrates and ammunition casings. 电沉积氧化还原材料,具有增强黄铜基材和弹壳上潜在手印可视化的潜力。
IF 2.6 3区 医学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2025-04-19 DOI: 10.1016/j.forc.2025.100663
Colm McKeever, Eithne Dempsey
Electrochemical methods can play a key role in the analysis of impression evidence, specifically, latent finger-marks on brass substrates and ammunition casings, the latter being commonly encountered at crime scenes in forensic casework. In adopting such techniques, forensic investigators can potentially overcome some of the challenges associated with traditional visualisation methods, the use of aggressive reagents, preservation of evidence integrity and the need for extensive sample preparation. The spatially selective deposition of conducting/redox active polymers for visualising latent finger-marks on typically low-yield brass ammunition casings is examined here, exploiting the electrodeposition of 3,4-ethylenedioxythiophene (EDOT), together with a first-time study of phenozine vs. phenothiazine monomers, and their combinations at sheet and cartridge brass. Fine tuning of electrochemical protocols and conditions together with optimised monomer feedstocks played a key role in the finger-mark visualisation quality achieved with insights into brass electrochemistry. EDOT-thionine emerged consistently as the most effective combination upon electrochemical deposition on brass sheets, revealing latent finger-marks (groomed) at the highest level of detail (level 3), including pores within the papillary ridges, using a low energy, rapid (t = 120 s) constant potential (Eapp = 0.1 V vs Ag|AgCl) approach. Successful visualisation of groomed and natural (donor) latent finger-marks was achieved following exposure of brass to temperatures of 700 °C and > 15-month room temperature aging. Bespoke electrochemical cells designed to facilitate the use of ammunition casings as working electrodes produced excellent results via potential sweeping, resulting in pristine visualised latent finger-marks (groomed) of grade 3 quality with visible level 3 (> 50 %) features.
电化学方法可以在分析印痕证据中发挥关键作用,特别是黄铜基材和弹壳上的潜在手印,后者在法医案件工作中经常在犯罪现场遇到。在采用这种技术时,法医调查人员可以潜在地克服与传统可视化方法、使用攻击性试剂、保存证据完整性以及需要大量样品制备有关的一些挑战。本文研究了导电/氧化还原活性聚合物的空间选择性沉积,用于在典型的低产量黄铜弹壳上观察潜在的手印,利用3,4-乙烯二氧噻吩(EDOT)的电沉积,以及首次研究了吩嗪与吩噻嗪单体,以及它们在片材和弹壳黄铜上的组合。电化学方案和条件的微调以及优化的单体原料在通过对黄铜电化学的深入了解实现手指印可视化质量方面发挥了关键作用。edot -硫氨酸作为电化学沉积在黄铜片上最有效的组合,在最高细节水平(3级)上显示潜在的手印(修饰),包括乳头状脊内的孔隙,使用低能,快速(t = 120 s)恒定电位(Eapp = 0.1 V vs Ag|AgCl)方法。在将黄铜暴露于700°C和>的温度下后,成功地可视化了修剪过的和天然的(供体)潜在手印。室温陈酿15个月。定制的电化学电池设计便于使用弹药外壳作为工作电极,通过潜在扫描产生优异的效果,产生3级质量的原始可见潜在手印(修饰),可见3级(>;50%)特征。
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引用次数: 0
Application of the expert algorithm for substance identification (EASI) to the electron ionization (EI) mass spectra of fentanyl isomers and analogs 物质鉴定专家算法(EASI)在芬太尼异构体和类似物电子电离质谱中的应用
IF 2.6 3区 医学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2025-04-09 DOI: 10.1016/j.forc.2025.100660
Alexandra I. Adeoye , Glen P. Jackson
Fentanyl analogs (fentalogs) share many structural and mass spectral similarities that make them difficult to differentiate and accurately identify without chromatographic data. In such situations, the expert algorithm for substance identification (EASI) provides superior classification relative to conventional approaches. Using a database of >57,000 replicate electron-ionization mass spectra of 76 fentalogs from ten laboratories, three challenging sets of isomers were studied in detail. To maximize limits of detection, only the 20 most abundant ions were considered. In each case, 50 % of the data from one laboratory served as the training set. On average, the mean absolute residuals between measured and modeled abundances of known positives were five times smaller using EASI than the consensus approach, which used the means of training sets as the exemplar spectra to which all query spectra were compared. With a conservative threshold of zero false positives, EASI identified isovalerylfentanyl from its two closest isomers with an accuracy of 96.7 %, which was ∼10 % better than the consensus approach. The associated positive likelihood ratios increased from 366 for the consensus approach to more than 4,200 for EASI. When discriminating isovalerylfentanyl spectra from the other 72 fentalogs, EASI provided errorless results with a positive likelihood ratio exceeding 50,000. For all 9 fentalogs, EASI outperformed the consensus approach and the use of Mahalanobis distance as a metric for identifying outliers. In the absence of retention time information, EASI improves confidence in drug identifications, enables inter-laboratory identifications, and reduces the need for acquiring concomitant spectra of standards.
芬太尼类似物(fentalogs)在结构和质谱上有许多相似之处,因此在没有色谱数据的情况下难以区分和准确识别。在这种情况下,物质鉴定专家算法(EASI)提供了优于传统方法的分类方法。利用来自十个实验室的 76 种芬太尼的 57,000 份重复电子电离质谱数据库,对三组具有挑战性的异构体进行了详细研究。为了最大限度地提高检测限,只考虑了 20 个最丰富的离子。在每种情况下,来自一个实验室的 50% 的数据作为训练集。使用 EASI 方法,已知阳性物的测量丰度与模型丰度之间的平均绝对残差比共识方法小五倍,共识方法使用训练集的平均值作为示范光谱,所有查询光谱都与之进行比较。在假阳性为零的保守阈值下,EASI 从两种最接近的异构体中识别出异戊酰芬太尼的准确率为 96.7%,比共识方法高出 10%。相关的阳性似然比从共识方法的 366 增加到 EASI 的 4,200 以上。在将异戊酰基芬太尼光谱与其他 72 种芬太尼进行鉴别时,EASI 提供了无差错的结果,其阳性似然比超过了 50,000 。在所有 9 种芬太尼中,EASI 的表现均优于共识方法和使用马哈拉诺比距离(Mahalanobis distance)作为识别异常值的指标的方法。在没有保留时间信息的情况下,EASI 提高了药物鉴定的可信度,实现了实验室之间的鉴定,并减少了获取标准品相关光谱的需要。
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引用次数: 0
Isotope fractionation during synthesis of methamphetamine from propiophenone, NaNO2 and dimethyl carbonate 丙烯酮、NaNO2和碳酸二甲酯合成甲基苯丙胺的同位素分馏
IF 2.6 3区 医学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2025-04-09 DOI: 10.1016/j.forc.2025.100661
Brendan M. Miller , James F. Carter , Sarah L. Cresswell , Wendy A. Loughlin , Peter N. Culshaw
Ephedrine remains a key precursor in the production of methamphetamine. A novel ephedrine-based route to methamphetamine involved the nitrosation of propiophenone to α-isonitrosopropiophenone, followed by catalytic hydrogenation to phenylpropanolamine (± − norephedrine). Cyclization-methylation of phenylpropanolamine to 3,4-dimethyl-5-phenyl-2-oxazolidinone using dimethyl carbonate, followed by basic hydrolysis or catalytic hydrogenolysis formed ephedrine or methamphetamine, respectively.
An investigation into the stable isotope fractionation during the synthesis of methamphetamine from propiophenone, NaNO2 and dimethyl carbonate was performed using isotope ratio mass spectrometry. A negative isotopic shift was observed for δ15N upon nitrosation of propiophenone to α-isonitrosopropiophenone, and a negative isotopic shift for δ2H during catalytic hydrogenation of α-isonitrosopropiophenone to phenylpropanolamine. Minimal change in δ13C was observed throughout the reaction until the methylation step with dimethyl carbonate, where a negative isotopic shift was observed.
The δ13C values for the methamphetamine presented in a similar range to methamphetamine reported in previous work where the norephedrine/norpseudoephedrine was prepared via different starting materials (benzaldehyde and nitroethane), confirming that similar δ13C values will result from fractionation during methylation with dimethyl carbonate regardless of the origin of the norephedrine/norpseudoephedrine. Chiral analysis confirmed methamphetamine to be racemic.
麻黄碱仍然是生产甲基苯丙胺的关键前体。以麻黄碱为基础的新型甲基苯丙胺生产工艺包括将苯丙酮亚硝化为 α-异亚硝基苯丙酮,然后催化加氢生成苯丙羟胺(± - 去甲麻黄碱)。使用碳酸二甲酯将苯丙羟胺环化-甲基化为 3,4-二甲基-5-苯基-2-恶唑烷酮,然后进行碱水解或催化氢化,分别生成麻黄碱或甲基苯丙胺。在将苯丙酮硝化成 α-异硝基苯丙酮的过程中,观察到 δ15N 发生了负同位素移动,在将α-异硝基苯丙酮催化氢化成苯丙羟胺的过程中,观察到 δ2H 发生了负同位素移动。在整个反应过程中,δ13C 的变化极小,直到与碳酸二甲酯发生甲基化反应时,才观察到负同位素位移。甲基苯丙胺的δ13C值与之前工作中报告的甲基苯丙胺的δ13C值范围相似,在之前的工作中,去甲麻黄碱/去甲伪麻黄碱是通过不同的起始原料(苯甲醛和硝基乙烷)制备的。手性分析证实甲基苯丙胺是外消旋的。
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引用次数: 0
Rescuing fluorescence with steric hindrance: Perylene diimide based powder for latent fingerprint imaging 具有空间位阻的挽救荧光:苝二亚胺基粉末用于潜在指纹成像
IF 2.6 3区 医学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2025-04-08 DOI: 10.1016/j.forc.2025.100662
Rajdeep Kaur, Navjot Kaur, Prabhpreet Singh
We reported sterically crowded perylene diimide for rescuing its solid-state fluorescence through functionalization with bulkier hydroxyphenyl benzothiazole (PH2). The PH2 has (i) λmax.at 620 nm; (ii) 28.8 % solid-state quantum yield and (iii) 100 % red colour purity calculated from CIE plot. PH2 adsorbed on silica nanoparticles was utilized as a fluorescent powder for the visualization of latent fingerprints on different porous, non-porous and curved surfaces using powder-dusting methods. The LFPs were subjected to laboratory conditions simulating those in the field such as aging, temperature, UV light and humidity and we successfully demonstrated the applicability of PH2-SiO2 powder for the development and visualization of ridge pattern from these degraded LFPs. We also aimed to recover LFPs from physical evidence by developing the LFPs with PH2-SiO2 followed by lifting of fingerprints using adhesive tape.
我们报道了空间拥挤的苝二亚胺通过与体积较大的羟基苯并噻唑(PH2)官能化来挽救其固态荧光。PH2具有(i) λmax。620nm;(ii) 28.8%的固体量子产率和(iii) 100%的红色纯度计算从CIE图。利用吸附在二氧化硅纳米颗粒上的PH2作为荧光粉,采用粉末除尘法对不同多孔、非多孔和曲面上的潜在指纹进行可视化。实验结果表明,在老化、温度、紫外光和湿度等实验室模拟条件下,PH2-SiO2粉末可用于降解lfp的脊状图案的形成和可视化。我们还试图通过用PH2-SiO2制备lfp,然后用胶带提取指纹,从物证中恢复lfp。
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Forensic Chemistry
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