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HPLC‐MS/MS combined with membrane‐protected molecularly imprinted polymer micro‐solid‐phase extraction for synthetic cathinones monitoring in urine
Author(s) -
SánchezGonzález Juan,
Odoardi Sara,
Bermejo Ana María,
Bermejo–Barrera Pilar,
Romolo Francesco Saverio,
Moreda–Piñeiro Antonio,
StranoRossi Sabina
Publication year - 2019
Publication title -
drug testing and analysis
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.065
H-Index - 54
eISSN - 1942-7611
pISSN - 1942-7603
DOI - 10.1002/dta.2448
Subject(s) - molecularly imprinted polymer , chromatography , ethylene glycol dimethacrylate , solid phase extraction , chemistry , divinylbenzene , extraction (chemistry) , detection limit , ammonium hydroxide , high performance liquid chromatography , elution , monomer , polymer , styrene , organic chemistry , selectivity , copolymer , methacrylic acid , catalysis
Synthetic cathinones are a type of drug belonging to group of new psychoactive substances (NPSs). The illicit market for these substances is characterized by the continuous introduction to the market of new analogs to evade legislation and to avoid detection. New screening and confirmation assays are therefore needed, mainly in forensic/clinical samples. In the current development, a porous membrane‐protected, micro‐solid‐phase extraction (μ‐SPE) has been developed for the assessment of several cathinones in urine. The μ‐SPE device consisted of a cone‐shaped polypropylene (PP) porous membrane containing the adsorbent (molecularly imprinted polymers, MIPs, synthesized for the first time for this class of drugs). MIPs were prepared using ethylone and 3‐methylmethcathinone (3‐MMC) as templates, ethylene glycol dimethacrylate (EGDMA) as a functional monomer, divinylbenzene (DVB) as a cross‐linker, and 2,2´‐azobisisobutyronitrile (AIBN) as an initiator. The prepared ethylone‐based MIP and 3‐MMC‐based MIP have been fully characterized and evaluated as new selective adsorbents for μ‐SPE. Cathinones separation/determination was performed by high performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS). Optimum loading conditions (pH 5.0, loading for 4.0 minutes under orbital‐horizontal shaking at 200 rpm) and elution conditions [2.0 mL of 75:20:5 heptane/2‐propanol/ammonium hydroxide and ultrasounds assistance (37 kHz, 325 W) for 4.0 minutes] were found for ethylone‐based MIP. Validation (intra‐day and inter‐day precision and analytical recovery) showed RSD values lower than 9 and 10% for intra‐day and inter‐day precision, and within the 88%–101% range for intra‐day and inter‐day analytical recovery.