Analysis of new psychoactive substances in oral fluids by means of microextraction by packed sorbent followed by ultra‐high‐performance liquid chromatography–tandem mass spectrometry

Abstract

In recent years, new drugs, commonly known as new psychoactive substances (NPS), appeared on the market, which include, among others, synthetic cannabinoids, cathinones, and tryptamine analogs of psilocin. The aim of this work was to develop and validate a new method for simultaneous screening and quantification of 31 NPS in oral fluid by ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The chosen target analytes represented different chemical and toxicological NPS classes, such as synthetic cathinones, piperazines, phenethylamines, synthetic cannabinoids, and their metabolites. The procedure involved a rapid sample preparation based on protein precipitation followed by clean-up utilizing microextraction by packed sorbent (MEPS); the quantitative analysis was performed by UHPLC-MS/MS. The MEPS clean-up, regardless of non-quantitative recoveries for some analytes, provided an effective removal of interfering compounds, as demonstrated by reduced matrix effects found at different concentrations for all the analytes. The validation protocol, based on SWGTOX guidelines, demonstrated the suitability of the proposed method for quantitative analysis: linearity range ranged over 3 or 4 orders of magnitude; precision and accuracy tests gave RSD% values below 25%, and accuracy ranged from 85.9% to 107%, accomplishing SWGTOX requirements. Limits of detection (LODs) ranged between 0.005 ng/mL and 0.850 ng/mL and limits of quantification (LOQs) from 0.015 to 2.600 ng/mL.

How to ask about the use of new psychoactive substances to increase the validity of results in self‐report prevalence surveys

“…There are general problems with the reliability of NPS survey data, given the number of substances on the market, recollection of rather technical terms, or lack of information about the substance. Further validation of self‐reported NPS use could include the testing of biological samples but would be limited by the analytical capacity to detect NPSs that are new on the market or the fact that NPSs have been increasingly found in illegal drug samples .…”

Recent applications of microextraction sample preparation techniques in biological samples analysis

“…They developed MEPS with ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Linearity ranged over 3 or 4 orders of magnitude; precision and accuracy tests gave RSD values <25%, and accuracy ranged from 85.9 to 107% (Rocchi et al, 2018).…”

“…The use of saliva samples in a study of 31 new psychoactive substances was reported by Rocchi et al (2018). They developed MEPS with ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS).…”

Validation of a Bioanalytical Method for the Determination of Synthetic and Natural Cannabinoids (New Psychoactive Substances) in Oral Fluid Samples by Means of HPLC-MS/MS

“…These substances have become a global phenomenon, with more than 120 countries and territories having reported at least one NPS (UNODC Early Warning Advisory on New Psychoactive Substances, 2020). In particular, until recently, 950 substances have been reported to the (UNODC) by governments, laboratories, and partner organizations (Rocchi et al, 2018; United Nations Office on Drugs Crime, 2019, 2020). Although synthetic cannabinoids are rapidly evolving and there are serious difficulties controlling them on the market (Coulter et al, 2011), in Europe, the European Monitoring Centre for Drugs and Drug Addiction (EMCDDA), through the EU Early Warning System, constantly monitors the use of synthetic cannabinoids.…”