Analysis of hydroxylated phenylalkylamine stimulants in urine by GC-APPI-HRMS
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RESEARCH PAPER
Analysis of hydroxylated phenylalkylamine stimulants in urine by GC-APPI-HRMS Claudia Bressan 1 & Juan F. Ayala-Cabrera 2 & Francisco Javier Santos 2 & Susana Cuadras 1 & Lorena Garrostas 1 & Núria Monfort 1 & Élida Alechaga 1 & Encarnación Moyano 2 & Rosa Ventura 1 Received: 18 May 2020 / Revised: 4 August 2020 / Accepted: 24 August 2020 / Published online: 21 September 2020 # Springer-Verlag GmbH Germany, part of Springer Nature 2020
Abstract A gas chromatography-atmospheric pressure photoionization-high-resolution mass spectrometry (GC-APPI-HRMS) method was developed for the determination of eight phenylalkylamine stimulants in urine samples. Spiked urine samples were hydrolyzed, processed by solid-phase extraction, and derivatized before analysis. Two derivatization reactions were studied: the formation of trimethylsilyl (TMS) derivatives with N-methyl-N-trimethylsilyl trifluoroacetamide (MSTFA) and trimethylsilyl/ trifluoroacetyl (TMS/TFA) derivatives with MSTFA and N-methyl-bis (trifluoroacetamide) (MBTFA) as derivatization reagents. Gas chromatography of both derivatives was performed with a 100% dimethylsiloxane column and a good separation of all isomeric compounds was achieved. To maximize the signal of the protonated molecule [M+H]+, the APPI most critical parameters were optimized. Three solvents were tested as dopant agents, with acetone yielding the lower in-source collision-induced dissociation (CID) fragmentation. The acquisition was performed in full scan and product ion scan (parallel reaction monitoring, PRM) using a quadrupole-Orbitrap mass analyzer (35,000 FWHM at m/z 200) in positive ion detection mode. At the optimal working conditions, the full scan method was evaluated for the fulfillment of identification requirements in doping analysis. Selectivity, limits of detection, matrix effect, and precision were estimated to validate the method for confirmation purposes and its applicability was tested by the analysis of spiked samples as well as by the analysis of samples obtained after the administration of some of the compounds to healthy volunteers. Results were compared with those obtained by GC-electron ionizationMS, demonstrating that the GC-APPI-HRMS method improved selectivity and sensibility, achieving lower limits of detection and satisfactory reproducibility. Keywords GC-APPI . Doping . Stimulants . TMS derivative . TMS/TFA derivative
Introduction The objective of anti-doping laboratories is to control the abuse of drugs that enhance the psycho-physical efficiency of athletes in sports. The analytical methods used to detect Electronic supplementary material The online version of this article (https://doi.org/10.1007/s00216-020-02913-0) contains supplementary material, which is available to authorized users. * Rosa Ventura [email protected] 1
Catalonian Antidoping Laboratory, Doping Control Research Group, IMIM (Hospital del Mar Medical Research Institute), Doctor Aiguader 88, 08003 Barcelona, Spain
2
Department of Chemical Engineering and Analytical Chemistry, Univers
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