title: High-throughput screening and quantitation of guanidino and ureido compounds using liquid chromatography-drift tube ion mobility spectrometry-mass spectrometry.
abstract: The present work focused on the high-throughput screening and quantitation of guanidino compounds (GCs) and ureido compounds (UCs) in human thyroid tissues. The strategy employed benzylic rearrangement stable isotope labeling (BRSIL) for the sample preparation and then detection using liquid chromatography-drift tube ion mobility spectrometry-quadrupole time of flight mass spectrometry (LC-DTIMS-QTOF MS). A short reversed-phase LC realized an on-line desalting and a measurement cycle of 5.0 min. DTIMS separation enhanced the better specificity and selectivity for the benzil labeled GCs and UCs. The elevated mass resolution of QTOF MS enabled measure of the characteristic ions at accurate mass in MS and tandem MS spectra. Collision cross section (CCS) from DTIMS and accurate mass from QTOF MS were used as two qualifiers for the profiling and identification of GCs and UCs. In addition, an integral abundance arising from 3-D ion features (retention time, drift time, m/z) was applied to quantify the GCs and UCs in human thyroid tissues. The quantitative validation indicated good linearity (coefficient values ≥ 0.9981), good precision (1.0%-12.3% for intra-day and 0.9%-7.8% for inter-day) and good accuracy (91%-109%). The results demonstrated that the developed BRSIL coupled with LC-DTIMS-QTOF MS can be a powerful analysis platform to investigate GCs and UCs in human thyroid tissues.
authors.affiliation: National Center for Organic Mass Spectrometry in Shanghai, Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, 345 Lingling Road, Shanghai 200032, People's Republic of China.
authors.forename: Ruo-Jing
authors.initials: RJ
authors.lastname: Fan
authors.affiliation: National Center for Organic Mass Spectrometry in Shanghai, Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, 345 Lingling Road, Shanghai 200032, People's Republic of China. Electronic address: fzhang@sioc.ac.cn.
authors.forename: Fang
authors.initials: F
authors.lastname: Zhang
authors.affiliation: National Center for Organic Mass Spectrometry in Shanghai, Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, 345 Lingling Road, Shanghai 200032, People's Republic of China.
authors.forename: Xiu-Ping
authors.initials: XP
authors.lastname: Chen
authors.affiliation: National Center for Organic Mass Spectrometry in Shanghai, Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, 345 Lingling Road, Shanghai 200032, People's Republic of China.
authors.forename: Wan-Shu
authors.initials: WS
authors.lastname: Qi
authors.affiliation: Department of Head and Neck Surgery, Fudan University Shanghai Cancer Center, Shanghai 200032, People's Republic of China; Department of Oncology, Shanghai Medical College, Fudan University, Shanghai 200032, People's Republic of China.
authors.forename: Qing
authors.initials: Q
authors.lastname: Guan
authors.affiliation: Department of Head and Neck Surgery, Fudan University Shanghai Cancer Center, Shanghai 200032, People's Republic of China; Department of Oncology, Shanghai Medical College, Fudan University, Shanghai 200032, People's Republic of China. Electronic address: tuanqisun@163.com.
authors.forename: Tuan-Qi
authors.initials: TQ
authors.lastname: Sun
authors.affiliation: National Center for Organic Mass Spectrometry in Shanghai, Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, 345 Lingling Road, Shanghai 200032, People's Republic of China. Electronic address: ylguo@sioc.ac.cn.
authors.forename: Yin-Long
authors.initials: YL
authors.lastname: Guo
mesh_terms: D002853:Chromatography, Liquid; D006146:Guanidines / Q000032:analysis*; D057166:High-Throughput Screening Assays; D006801:Humans; D000075663:Ion Mobility Spectrometry; D007553:Isotope Labeling; D013961:Thyroid Gland / Q000737:chemistry*; D014508:Urea / Q000031:analogs & derivatives*
chemical_list: D006146:Guanidines; D014508:Urea
keywords: Drift tube ion mobility spectrometry-mass spectrometry; Guanidino group; Quantification analysis; Stable isotope labeling; Ureido group