Instituto Nacional de Medicina Legal e Ciências Forenses - Delegação do Centro, Serviço de Química e Toxicologia Forenses, Largo da Sé Nova, 3000-213, Coimbra Portugal.
Centro de Investigação em Ciências da Saúde, Faculdade de Ciências da Saúde da Universidade da Beira Interior (CICS-UBI), Avenida Infante D. Henrique, 6201-506, Covilhã, Portugal.
J Anal Toxicol. 2020 Jan 7;44(1):92-102. doi: 10.1093/jat/bkz053.
The production and consumption of new psychoactive substances (NPSs) has been raising a major concern worldwide. Due to easy access and available information, many NPSs continue to be synthesized with an alarming increase of those available to purchase, despite all the control efforts created. A new analytical method was developed and validated to determine a group of phenethylamines and synthetic cathinones: cathinone, flephedrone, buphedrone, 4-MTA, α-PVP, methylone, 2C-P, ethylone, pentylone, MDPV and bromo-dragonFLY in whole blood. A mixed-mode solid phase extraction was applied to 250 μL of sample, and the extracts were derivatized with fast microwave technique before being analyzed by gas chromatography-mass spectrometry (GC-MS). The validation procedure followed the Scientific Working Group for Forensic Toxicology (SWGTOX) guidelines with parameters that included selectivity, linearity, limits of detection and quantification, intra- and inter-day precision and accuracy, recoveries and stability. The method presented linearity between 5 and 500 ng/mL for cathinone, buphedrone, 4-MTA, methylone, 2C-P and bromo-dragonFLY, 10-500 ng/mL for flephedrone, ethylone, pentylone and MDPV, and 40-500 ng/mL for α-PVP, with determination coefficients above 0.99 for all analytes. Recoveries ranged between 70.3% and 116.6%, and regarding intra- and inter-day precision, the relative mean errors were typically lower than 8.6%. The method was successfully applied to over 100 authentic samples from the Laboratory of Chemistry and Forensic Toxicology, Centre Branch, of the National Institute of Legal Medicine and Forensic Sciences, Portugal.
新精神活性物质（NPSs）的生产和消费在全球范围内引起了极大关注。由于易于获取和信息公开，尽管已经采取了各种控制措施，但仍有许多 NPSs 被不断合成，并可购买到的 NPSs 数量也在不断增加。本研究建立并验证了一种用于检测全血中苯乙胺类和合成卡西酮类物质的分析方法：卡西酮、苯甲酮、丁基酮、4-MTA、α-PVP、甲酮、2C-P、乙基酮、戊基酮、MDPV 和溴代飞龙。采用混合模式固相萃取法（SPE）提取 250 μL 样本，然后用快速微波衍生化技术对提取物进行衍生化，最后用气相色谱-质谱联用仪（GC-MS）进行分析。本方法的验证符合科学工作小组法医学毒理学（SWGTOX）的指导原则，包括选择性、线性、检测限和定量限、日内和日间精密度和准确度、回收率和稳定性。该方法在 5-500ng/mL 范围内对卡西酮、丁基酮、4-MTA、甲酮、2C-P 和溴代飞龙具有线性关系，在 10-500ng/mL 范围内对苯甲酮、乙基酮、戊基酮和 MDPV 具有线性关系，在 40-500ng/mL 范围内对 α-PVP 具有线性关系，所有分析物的相关系数均大于 0.99。回收率在 70.3%-116.6%之间，日内和日间精密度的相对平均误差通常低于 8.6%。该方法已成功应用于葡萄牙国家法医研究所化学和法医毒理学实验室中心分所的 100 多个真实样本。
