Centro de Química Estrutural, Institute of Molecular Sciences, Departamento de Química e Bioquímica, Faculdade de Ciências, Universidade de Lisboa, Campo Grande, 1749-016, Lisboa, Portugal.
BioISI - Biosystems & Integrative Sciences Institute, Faculdade de Ciências, Universidade de Lisboa, Campo Grande, 1749-016, Lisboa, Portugal.
Anal Bioanal Chem. 2024 Nov;416(28):6307-6316. doi: 10.1007/s00216-024-05517-0. Epub 2024 Sep 11.
In recent years, synthetic cannabinoids (SCs) have become a major public health issue. For this reason, there is a need for innovative analytical methods that allow its monitoring in biological matrices. In this work, we propose a novel methodology to screen eight SCs (AM-694, cumyl-5F-PINACA, MAM-2201, 5F-UR-144, JWH-018, JWH-122, UR-144 and APINACA) in oral fluids. A bar adsorptive microextraction method followed by microliquid desorption combined with high-performance liquid chromatography with diode array detection (BAµE-µLD/HPLC-DAD) was developed to monitor the target SCs. The main factors affecting the BAµE technology were fully optimized for oral fluid analysis. Under optimized experimental conditions, the proposed methodology showed good linear dynamic ranges from 20.0 to 2000.0 µg L (r > 0.99, relative residuals < 15%), limits of detection between 2.0 and 5.0 µg L and suitable average recovery yields (87.9-100.5%) for the eight studied SCs. The intra- and interday accuracies (bias ≤ ± 14.7%) and precisions (RSD ≤ 14.9%) were also evaluated at three spiking levels. The validated methodology was then assayed to oral fluid samples collected from several volunteers. The proposed analytical approach showed remarkable performance and could be an effective alternative for routine monitoring of the target compounds in oral fluid.
近年来,合成大麻素 (SCs) 已成为一个主要的公共卫生问题。出于这个原因,需要开发创新的分析方法来监测生物基质中的 SCs。在这项工作中,我们提出了一种新的方法来筛选八种 SCs(AM-694、cumyl-5F-PINACA、MAM-2201、5F-UR-144、JWH-018、JWH-122、UR-144 和 APINACA)在口腔液中的含量。建立了一种基于 bar 吸附微萃取(BAµE)和微液解吸(µLD)与高效液相色谱-二极管阵列检测联用(HPLC-DAD)的新方法,用于监测目标 SCs。对影响 BAµE 技术的主要因素进行了全面优化,以适用于口腔液分析。在优化的实验条件下,该方法在 20.0 至 2000.0 µg L 的范围内呈现出良好的线性动态范围(r > 0.99,相对残差 < 15%),检测限在 2.0 至 5.0 µg L 之间,对 8 种研究 SCs 的平均回收率在 87.9%至 100.5%之间。该方法的日内和日间精密度(偏差≤±14.7%)和准确度(回收率≤±14.9%)在三个加标水平下均得到了评估。然后,将该方法应用于从几名志愿者采集的口腔液样本中进行了检测。该分析方法具有良好的性能,可能成为常规监测口腔液中目标化合物的有效替代方法。