Determination of Synthetic Cathinones in Urine Using Gas Chromatography–Mass Spectrometry Techniques

Abstract

In recent years, the abuse of synthetic cathinones has increased considerably. This study proposes a method, based on gas chromatography/mass spectrometry (GC-MS), to analyze and quantify six synthetic cathinones in urine samples: mephedrone (4-MMC), methylone (bk-MDMA), butylone, ethylone, pentylone and methylenedioxypyrovalerone (MDPV). In our procedure, the urine samples undergo solid-phase extraction (SPE) and derivatization prior to injection into the GC-MS device. Separation is performed using a HP-5MS capillary column. The use of selective ion monitoring (SIM mode) makes it is good sensitivity in this method, and the entire analysis process is within 18 min. In addition, the proposed method maintains linearity in the calibration curve from 50 to 2,000 ng/mL (r(2) > 0.995). The limit of detection of this method is 5 ng/mL, with the exception of MDPV (20 ng/mL); the limit of quantification is 20 ng/mL, with the exception of MDPV (50 ng/mL). In testing, the extraction performance of SPE was between 82.34 and 104.46%. Precision and accuracy results were satisfactory <15%. The proposed method was applied to six real urine samples, one of which was found to contain 4-MMC and bk-MDMA. Our results demonstrate the efficacy of the proposed method in the identification of synthetic cathinones in urine, with regard to the limits of detection and quantification. This method is highly repeatable and accurate.

Analytical quantification, intoxication case series, and pharmacological mechanism of action for N‐ethylnorpentylone (N‐ethylpentylone or ephylone)

“…N-Ethylnorpentylone is a synthetic cathinone that is being encountered in recreational drug markets worldwide, yet little is known about its toxicology or pharmacology. 26,27 Numerous analytical methods are published describing analyses of synthetic cathinones in biological samples, [31][32][33][34][35][36][37] but only two articles have reported quantitation of N-ethylnorpentylone. 26,27 Here we present a fully validated method to detect and quantify this substance in whole blood.…”

GC–MS Quantification Method for Mephedrone in Plasma and Urine: Application to Human Pharmacokinetics

“…With gas chromatography-mass spectrometry (GC-MS) a technique based on a solid-phase extraction (SPE) has been reported (13). With liquid chromatography tandem mass spectrometry (LC-MS/MS) mephedrone was detected in several matrices such as dried blood spots, dried plasma, urine, oral fluid, and hair (14)(15)(16)(17).…”

“…With liquid chromatography tandem mass spectrometry (LC-MS/MS) mephedrone was detected in several matrices such as dried blood spots, dried plasma, urine, oral fluid, and hair (14)(15)(16)(17). Most of the available literature is limited to case reports of intoxications, screenings, and post-mortem analyses (11)(12)(13)(14)(15)(16)(17)(18)(19)(20).…”

3,4-Methylenedioxypyrovalerone (MDPV) Sensing Based on Electropolymerized Molecularly Imprinted Polymers on Silver Nanoparticles and Carboxylated Multi-Walled Carbon Nanotubes

“…Currently, there are several methods in literature for MDPV quantification ( Table 1 ). They are mainly based on liquid chromatography (LC) associated to a mass spectrometry (MS) detector [ 25 , 26 , 27 , 28 , 29 , 30 , 31 , 32 , 33 , 34 , 35 , 36 , 37 ], gas chromatography (GC) associated with MS [ 38 , 39 , 40 , 41 , 42 , 43 , 44 ] or flame ionization detection (FID) [ 41 ]. There are a few works with other techniques, like ion mobility spectrometry subsequent to liquid-liquid extraction [ 45 ], capillary electrophoresis (CE) with in-line solid-phase extraction (SPE) and spectrophotometric detection [ 46 ], Raman spectroscopy [ 47 ], nuclear magnetic resonance (NMR) spectroscopy [ 48 ] and direct MS analysis [ 49 ]; there is also a commercially available portable immunoassay [ 50 ].…”