Abstract

Methyl 2 -[ [ 1- (5- fluoropentyl) indole - 3- carbonyl] amino] -3, 3- dimethyl - butanoate (5F-MDMB-PICA) is a new synthetic cannabinoid characterized by valinate or tert-leucinate moieties. In recent years, 5F-MDMB-PICA has been abused in the form of “spice-like” herbal incenses or electronic cigarette oil. A UHPLC-MS/MS method was developed to detect 5F-MDMB-PICA and its metabolites in human hair. Approximately 20 mg of hair was weighed and pulverized with methanol below 4°C. After ultrasonication, centrifugation and filtration, 200 μL of supernatant was placed into an autosampler vial and analyzed on a Waters Acquity UPLC HSS T3 column (100 mm × 2.1 mm, 1.8 μm particle size) using an acetonitrile-20 mmol/L ammonium acetate (0.1% formic acid, 5% acetonitrile) gradient with a run time of 8 min. The limit of detection (LOD) ranged from 0.5 to 5 pg/mg, and the lower limit of quantitation (LLOQ) ranged from 1 to 5 pg/mg. The method was shown to be linear over a concentration range of 1–200 pg/mg. The linear correlation (R2) of the calibration curves for all analytes was >0.999. The accuracy varied from 95.4 to 107.4%, while the intra- and inter-day precision RSD values were 0.7–10.6% and 1.7–12.2%, respectively. Recoveries were within the range of 61.1–93.3%, and matrix effects were in the range of 19.1–102.6%. The validated method was successfully applied to the identification and quantification of 5F-MDMB-PICA and its metabolites in hair from authentic forensic cases.

Highlights

  • New psychoactive substances (NPS) have surged at an alarming rate worldwide, which has severely impacted global health problems

  • There have been some reports in the literature on the choice of organic solvents to extract synthetic cannabinoids in hair (Hutter et al, 2012; Salomone et al, 2012, 2014; Gottardo et al, 2014), methanol is the most common solvent for extracting drugs from hair

  • To obtain a good extraction recovery and absence of a significant matrix effect, 5F-MDMB-PICA and its metabolites were filtered with different filter membranes

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Summary

INTRODUCTION

New psychoactive substances (NPS) have surged at an alarming rate worldwide, which has severely impacted global health problems. Methyl 2-[[1-(5-fluoropentyl)indole-3-carbonyl]amino]-3,3dimethyl-butanoate (5F-MDMB-PICA) belongs to the class of synthetic cannabinoids. This compound was synthesized and described for the first time by Banister et al for the purpose of pharmacological research on novel SCs characterized by valinate or tert-leucinate moieties (Banister et al, 2016). Only the detection of 5F-MDMB-PICA and its metabolites in urine have been reported (Mogler et al, 2018; Truver et al, 2020). Synthetic cannabinoids are usually monitored by analyzing the parent drug and its metabolites in blood and urine samples (Presley et al, 2016; Krotulski et al, 2019). A validated method is presented for the quantitative determination of 5F-MDMBPICA and its five metabolites in human hair by liquid chromatography-tandem mass spectrometry (Scheme 1). The method was successfully applied to authentic hair samples from real cases

MATERIALS AND METHODS
C24 H18 D5 NO2
Method Development
CONCLUSION
DATA AVAILABILITY STATEMENT

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