Analysis of Selective Androgen Receptor Modulators by Gas Chromatography-Microchip Atmospheric Pressure Photoionization-Mass Spectrometry

作者：Luosujarvi Laura^*; Haapala Markus; Thevis Mario; Saarela Ville; Franssila Sami; Ketola Raimo A; Kostiainen Risto; Kotiaho Tapio

来源：Journal of the American Society for Mass Spectrometry, 2010, 21(2): 310-316.

DOI：10.1016/j.jasms.2009.10.019

A gas chromatography-microchip atmospheric pressure photoionization-mass spectrometric (GC-mu APPI-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(+center dot)) and protonated molecules ([M + H](+)) in photoionization. Better signal-to-noise ratios (S/N) were obtained in MS/MS analysis using the M(+center dot) ions as precursor ions than using the [M + H](+) ions, and therefore the M(+center dot) 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-mu APPI-MS study, the proof-of-principle of gas chromatography-microchip atmospheric pressure chemicalionization-Orbitrap MS (GC-mu APCI-Orbitrap MS) was demonstrated.

• 出版日期2010-2