Simultaneous quantitation of synthetic cathinone positional isomers in wastewater and urine using liquid chromatography-high-resolution mass spectrometry.

Abstract

Over the past decade, an alarming number of new compounds (NPSs) have emerged in the recreational drug market, posing serious threats to both public health and society. Many NPSs are positional isomers or structurally related compounds of illegal substances, which potentially harm public health due to their largely unknown pharmacological and toxicological effects, leading to tremendous demand for powerful and effective NPS screening methods. Synthetic cathinones (SCs) are the second most prevalent class of NPSs in Europe, a class encompassing a large number of isomers, showing the need for adequate analytical approaches to discriminate them. Urine testing is typically used to detect NPSs, with samples obtained through a non-invasive sampling technique. In addition, wastewater analysis provides a complementary method to monitor community-level trends in the use of these rapidly evolving substances. This study presents the development and validation of an analytical method based on solid-phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the simultaneous separation and quantitation of three sets of synthetic cathinone positional isomers, namely, chloromethcathinone, methylones, and ethylones in both wastewater and urine matrices. An LC-MS/MS method using high-resolution multiple reaction monitoring (MRMHR) acquisition was developed for the analysis of spiked wastewater and urine matrices, and its analytical performance was compared with that of high-resolution selected ion monitoring (HR-SIM). The developed method was validated in terms of selectivity, linearity and range, precision, accuracy, limit of detection, and lowest limit of quantification. Recovery and matrix effects were also assessed. The lower limits of quantification (LLOQs) for all seven compounds were as low as 0.1 ng mL-1 in both matrices. The developed method provides a validated analytical framework for the selective separation and quantitation of synthetic cathinone positional isomers in urine and wastewater matrices.

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