High-Throughput LC–MS/MS Based Simultaneous Determination of Polyamines Including N-Acetylated Forms in Human Saliva and the Diagnostic Approach to Breast Cancer Patients

• DOI: 10.1021/ac402526c
• Publication Date: 2013-11-15T00:04:03Z
• Authors: Haruhito Tsutsui; Toshiki Mochizuki; Koichi Inoue; Tatsuya Toyama; Nobuyasu Yoshimoto; Yumi Endo; Kenichiro Todoroki; Jun Zhe Min; Toshimasa Toyo’oka
• Keywords: Sulfonamides; Time Factors; Acetylation; Breast Neoplasms; 01 natural sciences; 0104 chemical sciences; 3. Good health; Tandem Mass Spectrometry; Case-Control Studies; Polyamines; Saliva; Oxazoles; Chromatography, Liquid

The determination of polyamines and their N-acetylated forms was performed by ultraperformance liquid chromatography coupled with tandem mass spectrometry (UPLC–MS/MS). efficiently reacted 4-(N,N-dimethylaminosulfonyl)-7-fluoro-2,1,3-benzoxadiazole (DBD-F) in 0.1 M borax (pH 9.3) at 60 °C for 30 min. resulting derivatives were analyzed electrospray ionization (ESI)-MS sensitively detected selected reaction monitoring (SRM). Furthermore, a rapid separation the polyamine within 10 min UPLC using an antipressurized column packed 1.7-μm octadecylsilyl (ODS) silica gel. limits detection (S/N = 3) on SRM chromatograms attomole level (9–43 amol). This procedure used to successfully determine 11 polyamines, including forms, saliva patients primary relapsed breast cancer healthy volunteers. several (Ac-PUT, Ac-SPD, Ac-SPM, DAc-SPD, DAc-SPM) increases patients. levels three (Ac-SPM, significantly higher only present method proved highly sensitive is characterized specificity feasibility sample analysis. Consequently, proposed useful noninvasive salivary diagnosis could be applied specimens biological nature.