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Pressurized liquid extraction for the determination of cannabinoids and metabolites in hair: Detection of cut-off values by high performance liquid chromatography-high resolution tandem mass spectrometry

机译:加压液体萃取法测定头发中的大麻素和代谢物:高效液相色谱-高分辨率串联质谱法检测临界值

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Hair analysis has become a routine procedure in most forensic laboratories since this alternative matrix presents clear advantages over classical matrices; particularly wider time window, non-invasive sampling and good stability of the analytes over time. There are, however, some major challenges for the analysis of cannabinoids in hair, mainly related to the low concentrations of 11-nor-9-carboxy-Delta(9)-tetrahydrocannabinol (THC-COOH), that is the major metabolite. In this study a fast, accurate and sensitive method for the determination of cannabinol, cannabidiol, THC and THC-COOH in hair has been developed. The extraction of analytes from hair (50 mg) is based on an automated pressurized liquid extraction (PLE) using water modified with the surfactant sodium dodecyl sulphate as eluent phase. PLE extract is then cleaned up by SPE using polymeric reversed phase cartridges Strata XL before the injection in the HPLC-HRMS/MS system. Chromatographic conditions obtained with a fused-core column allowed a good separation of the analytes in less than 4 min. The whole procedure has been validated according to SWG-TOX guidelines. The LLOQs obtained for THC-COOH and the other analytes were respectively 0.1 and 2 pg/mg. To the best of our knowledge, this is the first LC-MS/MS based method that allows the detection of THC-COOH in hair at values lower than the cut-off. (C) 2015 Elsevier B.V. All rights reserved.
机译:毛发分析已成为大多数法医实验室的常规程序,因为这种替代性基质比传统基质具有明显优势。特别是更宽的时间范围,无创采样以及分析物随时间变化的良好稳定性。但是,分析头发中的大麻素存在一些主要挑战,主要与低浓度的11-nor-9-羧基-Delta(9)-四氢大麻酚(THC-COOH)有关,后者是主要的代谢产物。在这项研究中,开发了一种快速,准确和灵敏的测定头发中大麻酚,大麻二酚,THC和THC-COOH的方法。从头发(50 mg)中分析物的提取是基于自动加压液体提取(PLE),使用表面活性剂十二烷基硫酸钠改性的水作为洗脱液。然后在注入HPLC-HRMS / MS系统之前,使用聚合物反相小柱Strata XL通过SPE纯化PLE提取物。用熔融核色谱柱获得的色谱条件可在不到4分钟的时间内将分析物很好地分离。整个过程已根据SWG-TOX指南进行了验证。 THC-COOH和其他分析物的LLOQ分别为0.1和2 pg / mg。据我们所知,这是第一个基于LC-MS / MS的方法,该方法可以检测出低于临界值的头发中的THC-COOH。 (C)2015 Elsevier B.V.保留所有权利。

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