Microextraction by packed sorbent for the determination of selected synthetic cathinones and 2C-P in hair

IF 6.5 Q1 CHEMISTRY, ANALYTICAL Advances in Sample Preparation Pub Date : 2025-03-14 DOI:10.1016/j.sampre.2025.100175
Ana Y. Simão , Luana M. Rosendo , Pedro Dinis , Cláudia Margalho , Maristela Andraus , Mário Barroso , Eugenia Gallardo
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Abstract

New psychoactive substances (NPS), including synthetic cathinones and phenethylamines, pose significant challenges due to their evolving chemical structures and health impacts. This study aimed to optimize and validate a methodology for detecting and quantifying a number of synthetic cathinones [methylone, ethylone, pentedrone, 4-chloroethcathinone (4-CEC), penthylone, α-pyrrolidinopentiophenone (α-PVP), 3,4-methylenedioxypyrovalerone (MDPV), 4‑chloro-α-pyrrolidinovalerophenone (4-Cl-α-PVP), as well as phenethylamine 2,5-dimethoxy-4(n)-propylphenethylamine (2C-P)], in hair samples using microextraction by packed sorbent (MEPS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). We developed an environmentally friendly and cost-effective MEPS procedure, which was validated for selectivity, linearity, precision, accuracy, and recovery. Results demonstrated that the method effectively detects analytes with limits of quantification as low as 10 pg/mg. The method successfully identifies MDPV in concentrations consistent with those observed in chronic and acute drug consumption cases, proving its suitability in forensic and clinical toxicology. This approach offers a robust solution for forensic and clinical applications, by combining efficient sample clean-up with precise analytical capabilities.

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填充吸附剂微萃取法测定头发中合成卡西酮和2C-P的含量
新型精神活性物质(NPS),包括合成卡西酮和苯乙胺,由于其化学结构不断演变和对健康的影响,构成了重大挑战。本研究旨在优化和验证一种检测和定量合成卡西酮[甲酮、乙炔、戊酮、4-氯卡西酮(4- cec)、戊酮、α-吡咯烷二酮(α-PVP)、3,4-亚甲基二氧基戊酮(MDPV)、4-氯-α-吡咯烷二酮(4- cl -α-PVP)和苯乙胺2,5-二甲氧基-4(n)-丙基苯乙胺(2C-P)]的方法。利用填充吸附剂(MEPS)微萃取和液相色谱-串联质谱(LC-MS/MS)对头发样品进行分析。我们开发了一种环境友好且经济高效的MEPS程序,并对其选择性、线性度、精密度、准确度和回收率进行了验证。结果表明,该方法可有效检测分析物,定量限低至10 pg/mg。该方法成功地鉴定出MDPV浓度与慢性和急性吸毒病例中观察到的浓度一致,证明了其在法医和临床毒理学上的适用性。这种方法结合了高效的样品清理和精确的分析能力,为法医和临床应用提供了强大的解决方案。
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