Sánchez-González Juan, Odoardi Sara, Bermejo Ana María, Bermejo-Barrera Pilar, Romolo Francesco Saverio, Moreda-Piñeiro Antonio, Strano-Rossi Sabina
Group of Trace Elements, Spectroscopy, and Speciation (GETEE), Health Research Institute of Santiago de Compostela (IDIS), Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, Universidade de Santiago de Compostela, Santiago de Compostela, Spain.
Institute of Public Health, Section of Legal Medicine, Università Cattolica del Sacro Cuore, Rome, Italy.
Drug Test Anal. 2019 Jan;11(1):33-44. doi: 10.1002/dta.2448. Epub 2018 Sep 5.
Synthetic cathinones are a type of drug belonging to group of new psychoactive substances (NPSs). The illicit market for these substances is characterized by the continuous introduction to the market of new analogs to evade legislation and to avoid detection. New screening and confirmation assays are therefore needed, mainly in forensic/clinical samples. In the current development, a porous membrane-protected, micro-solid-phase extraction (μ-SPE) has been developed for the assessment of several cathinones in urine. The μ-SPE device consisted of a cone-shaped polypropylene (PP) porous membrane containing the adsorbent (molecularly imprinted polymers, MIPs, synthesized for the first time for this class of drugs). MIPs were prepared using ethylone and 3-methylmethcathinone (3-MMC) as templates, ethylene glycol dimethacrylate (EGDMA) as a functional monomer, divinylbenzene (DVB) as a cross-linker, and 2,2´-azobisisobutyronitrile (AIBN) as an initiator. The prepared ethylone-based MIP and 3-MMC-based MIP have been fully characterized and evaluated as new selective adsorbents for μ-SPE. Cathinones separation/determination was performed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Optimum loading conditions (pH 5.0, loading for 4.0 minutes under orbital-horizontal shaking at 200 rpm) and elution conditions [2.0 mL of 75:20:5 heptane/2-propanol/ammonium hydroxide and ultrasounds assistance (37 kHz, 325 W) for 4.0 minutes] were found for ethylone-based MIP. Validation (intra-day and inter-day precision and analytical recovery) showed RSD values lower than 9 and 10% for intra-day and inter-day precision, and within the 88%-101% range for intra-day and inter-day analytical recovery.
合成卡西酮是一类属于新型精神活性物质（NPS）的药物。这些物质的非法市场的特点是不断有新的类似物进入市场，以规避立法并避免被检测到。因此，主要在法医/临床样本中需要新的筛查和确证分析方法。在当前的研究中，已开发出一种多孔膜保护的微固相萃取（μ-SPE）方法，用于评估尿液中的几种卡西酮。μ-SPE装置由一个锥形聚丙烯（PP）多孔膜组成，该膜含有吸附剂（分子印迹聚合物，MIPs，首次针对此类药物合成）。使用乙酮和3-甲基甲卡西酮（3-MMC）作为模板、乙二醇二甲基丙烯酸酯（EGDMA）作为功能单体、二乙烯基苯（DVB）作为交联剂以及2,2´-偶氮二异丁腈（AIBN）作为引发剂制备MIPs。所制备的基于乙酮的MIP和基于3-MMC的MIP已被充分表征，并被评估为用于μ-SPE的新型选择性吸附剂。卡西酮的分离/测定通过高效液相色谱-串联质谱（HPLC-MS/MS）进行。发现基于乙酮的MIP的最佳上样条件为（pH 5.0，在200 rpm的水平轨道振荡下上样4.0分钟）和洗脱条件[2.0 mL的75:20:5庚烷/2-丙醇/氢氧化铵，并进行4.0分钟的超声辅助（37 kHz，325 W）]。验证（日内和日间精密度以及分析回收率）显示，日内和日间精密度的相对标准偏差（RSD）值低于9%和10%，日内和日间分析回收率在88%-101%范围内。
