Analysis of selective androgen receptor modulators by gas chromatography-microchip atmospheric pressure photoionization-mass spectrometry |
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Authors: | Laura Luosujärvi Markus Haapala Mario Thevis Ville Saarela Sami Franssila Raimo A Ketola Risto Kostiainen Tapio Kotiaho |
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Institution: | 1.Laboratory of Analytical Chemistry, Department of Chemistry,University of Helsinki,Helsinki,Finland;2.Division of Pharmaceutical Chemistry, Faculty of Pharmacy,University of Helsinki,Helsinki,Finland;3.Center for Preventive Doping Research—Institute of Biochemistry,German Sport University Cologne,Cologne,Germany;4.Department of Micro and Nanosciences,Helsinki University of Technology,Helsinki,Finland;5.Center for Drug Research, Faculty of Pharmacy,University of Helsinki,Helsinki,Finland |
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Abstract: | A gas chromatography-microchip atmospheric pressure photoionization-mass spectrometric (GC-μAPPI-MS) method was developed and used for the analysis of three 2-quinolinone-derived selective androgen receptor modulators
(SARMs). SARMs were analyzed from spiked urine samples, which were hydrolyzed and derivatized with N-methyl-N-(trimethylsilyl)trifluoroacetamide before analysis. Trimethylsilyl derivatives of SARMs formed both radical cations (M+•) and protonated molecules (M + H]+) in photoionization. Better signal-to-noise ratios (S/N) were obtained in MS/MS analysis using the M+• ions as precursor ions than using the M + H]+ ions, and therefore the M+• ions were selected for the precursor ions in selected reaction monitoring (SRM) analysis. Limits of detection (LODs) with
the method ranged from 0.01 to 1 ng/mL, which correspond to instrumental LODs of 0.2–20 pg. Limits of quantitation ranged
from 0.03 to 3 ng/mL. The mass spectrometric response to the analytes was linear (R ≥ 0.995) from the LOQ concentration level
up to 100 ng/mL concentration, and intra-day repeatabilities were 5%–9%. In addition to the GC-μAPPI-MS study, the proof-of-principle of gas chromatography-microchip atmospheric pressure chemical ionization-Orbitrap MS
(GC-μAPCI-Orbitrap MS) was demonstrated. |
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