Department of Chemistry, Tabriz Branch, Islamic Azad University, Tabriz, Iran.
Department of Chemistry, Tabriz Branch, Islamic Azad University, Tabriz, Iran.
J Chromatogr A. 2022 May 10;1670:462989. doi: 10.1016/j.chroma.2022.462989. Epub 2022 Mar 21.
The recognition of opioids, either as prescription drugs or illicit narcotics, is one of the hot challenges in the analytical field, especially in forensic medicine. Here, a rapid and high efficient air-assisted dispersive liquid-liquid microextraction (DLLME) running after a dispersive magnetic solid-phase extraction (MSPE) is developed for simultaneous extraction and preconcentration of tramadol and methadone in urine samples prior to gas chromatography-mass spectrometry (GC-MS) determination technique. The samples were first mixed with a new magnetic and porous adsorbent, based on a metal-organic framework (MOF) derived NH-functionalized FeO nanoparticles-carbon nanocomposite (NH-FeO@C). Then, the eluent, containing the retrieve analytes, was directly applied as the disperser solvent, along with dichloromethane extracting solvents, to perform DLLME. The combination of MSPE, using the new high surface area sorbent, with a high-performance DLLME resulted in exceptional enrichment factors and extraction recoveries. Under the optimized conditions, linear ranges of 0.1-30 ng mL and 0.1-35 ng mL, and detection limits of 73 and 32 pg mL, were obtained for tramadol and methadone, respectively. The developed system was utilized for the extraction and preconcentration of tramadol and methadone in some urine samples of suspected drug users, with a reasonable reproducibility (2.4-4.5%). The results were in good agreement with those of the official HPLC/MS-MS technique.
阿片类药物（无论是处方药物还是非法麻醉剂）的识别是分析领域，特别是法医学领域的一个热点挑战。在这里，开发了一种快速高效的空气辅助分散液液微萃取（DLLME），在分散磁性固相萃取（MSPE）之后，用于在气相色谱-质谱（GC-MS）测定技术之前同时提取和预浓缩尿液样品中的曲马多和美沙酮。样品首先与一种基于金属有机骨架（MOF）衍生的 NH 功能化 FeO 纳米粒子-碳纳米复合材料（NH-FeO@C）的新型磁性多孔吸附剂混合。然后，含有回收分析物的洗脱液直接用作分散溶剂，与二氯甲烷萃取溶剂一起用于 DLLME。MSPE 与使用新型高表面积吸附剂的高性能 DLLME 的结合，实现了出色的富集因子和提取回收率。在优化条件下，曲马多和美沙酮的线性范围分别为 0.1-30ng/mL 和 0.1-35ng/mL，检测限分别为 73 和 32pg/mL。所开发的系统用于提取和预浓缩一些疑似吸毒者的尿液样品中的曲马多和美沙酮，具有合理的重现性（2.4-4.5%）。结果与官方 HPLC/MS-MS 技术一致。
