UHPLC-HRMS and GC-MS Screening of a Selection of Synthetic Cannabinoids and Metabolites in Urine of Consumers

Abstract

Background and Objectives: The use of synthetic cannabinoids has increased around the world. As a result, the implementation of accurate analysis in human biological matrices is relevant and fundamental. Two different analytical technologies, ultra-high-performance liquid chromatography-high-resolution mass spectrometry (UHPLC-HRMS) and high-sensitivity gas chromatography-mass spectrometry (GC-MS) were used for the determination of three synthetic cannabinoids JWH-122, JWH 210, UR-144 and their metabolites in urine of consumers. Materials and Methods: Sample preparation included an initial hydrolysis with β-glucuronidase and liquid-liquid extraction. The UHPLC-HRMS method included a Kinetex 2.6 u Biphenyl 100A (100 × 2.1 mm, 2.6 μm) (Phenomenex, Italy) column with a gradient mobile phase consisting of mobile phase A (ammonium formate 2mM in water, 0.1% formic acid) and mobile phase B (ammonium formate 2mM in methanol/acetonitrile 50:50 (v/v), 0.1% formic acid) and a full-scan data-dependent MS2 (ddMS2) mode was used (mass range 100–1000 m/z). The GC-MS method employed an ultra-Inert Intuvo GC column (HP-5MS UI, 30 m × 250 µm i.d, film thickness 0.25 µm; Agilent Technologies, Santa Clara, CA, USA) and electron-impact (EI) mass spectra were recorded in total ion monitoring mode (scan range 40–550 m/z). Results: Both methods have been successfully used for screening of parent synthetic cannabinoids and their metabolites in urine samples of consumers. Conclusions: The screening method applied JWH-122, JWH-210, UR-144 and their metabolites in urine of consumers can be applied to other compounds of the JWH family.

Ultra-High Performance Liquid Chromatography-High Resolution Mass Spectrometry and High-Sensitivity Gas Chromatography-Mass Spectrometry Screening of Classic Drugs and New Psychoactive Substances and Metabolites in Urine of Consumers

“…The principal limitation of the presented methodology was the difficulty associated with data processing to get the information from single sample analysis that required qualified expertise. Moreover, in some cases it can be extremely difficult to chromatographically separate certain NPS to facilitate identification via mass spectrometry, such as in the case of isomers and isobaric compounds which display the same or significantly related chemical formulae [ 22 , 28 , 29 , 30 , 31 , 32 ].…”

“…Isomeric and isobaric substances require gas or liquid chromatographic conditions that enable adequate separation of the compounds prior to MS analysis or include other mass spectrometry data such as m / z , isotope pattern, retention time and fragmentation information [ 22 , 30 , 31 , 32 ].…”

Determination of the Synthetic Cannabinoids JWH-122, JWH-210, UR-144 in Oral Fluid of Consumers by GC-MS and Quantification of Parent Compounds and Metabolites by UHPLC-MS/MS

“…We here present, for the first time, two complementary analytical methods for the determination of JWH-122, JWH-210 and UR-144 in OF of consumers. As reported above, we focused on these particular substances due to their recent spread on the Spanish illegal market [ 26 ].…”

“…Representative chromatograms obtained following the extraction of 400 µL blank OF samples spiked with 1 and 0.5 ng/mL analytes under investigation for GC-MS and UHPLC-HRMS methods, respectively are reported in Figures 1 and 2 consumers OF after a single smoking self-administration. We focused on these particular substances due to their recent spread on the Spanish illegal market, as reported by the same consumers in web fora and to a Spanish non-governmental organization dealing with drug risk reduction, presenting several described adverse effects [26][27][28][29].…”

“…In this regard, we focused on the development and validation of two analytical methods for SCc determination in OF: a last generation gas chromatography–mass spectrometry (GC-MS) method for an initial target analysis of JWH-122, JWH-210 and UR-144 in consumers OF and then an ultra-high performance liquid chromatography high resolution mass spectrometry (UHPLC-HRMS) method for a complementary measurement of JWH-122, JWH-210, UR-144 and their metabolites time course in consumers OF after a single smoking self-administration. We focused on these particular substances due to their recent spread on the Spanish illegal market, as reported by the same consumers in web fora and to a Spanish non-governmental organization dealing with drug risk reduction, presenting several described adverse effects [ 26 , 27 , 28 , 29 ].…”