High‐temperature high‐performance liquid chromatography on a porous graphitized carbon column coupled to an Orbitrap mass spectrometer with atmospheric pressure photoionization for screening exogenous anabolic steroids in human urine

Abstract

The proposed method matches the basic requirements of all methods used to analyze drugs or metabolites in an antidoping laboratory, i.e., sensitivity, selectivity, and specificity. The acquisition of full-scan mass spectra with accurate masses can be a valuable tool in the retrospective evaluation of analyzed samples for anabolic steroids recently added to the prohibited list.

Annual banned‐substance review: analytical approaches in human sports drug testing

“…Combining high‐temperature LC employing a porous graphitized carbon column interfaced via an atmospheric pressure photoionization (APPI) source to a high resolution/high accuracy orbitrap analyzer was shown to allow for the sensitive analysis of 57 steroidal compounds from human urine . Using an approach based on enzymatic hydrolysis followed by liquid‐liquid extraction (LLE), target analytes were separated at 90 °C by means of the aforementioned graphitized carbon analytical column (100 x 1.0 mm, 3 µm particle size).…”

“…[51] Using one non-deuterated and three deuterated ISTDs, 0.5 mL of urine was solid-phase extracted (using a C-18-based adsorbent) and the target analytes Combining high-temperature LC employing a porous graphitized carbon column interfaced via an atmospheric pressure photoionization (APPI) source to a high resolution/high accuracy orbitrap analyzer was shown to allow for the sensitive analysis of 57 steroidal compounds from human urine. [52] Using an approach based on enzymatic hydrolysis followed by liquid-liquid extraction (LLE), target analytes were separated at 90°C by means of the aforementioned graphitized carbon analytical column (100 x 1.0 mm, 3 μm particle size). With 0.1% trifluoroacetic acid (solvent A) and acetonitrile/2-propanol (containing 0.1% trifluoroacetic acid, solvent B) gradient elution was completed in 20 min, diverting the analytes into the mass spectrometer operated in positive ionization full scan mode (resolution set to 60 000 FWHM).…”

Separation of Triacylglycerols from Edible Oil Using a Liquid Chromatography–Mass Spectrometry System with a Porous Graphitic Carbon Column and a Toluene–Isopropanol Gradient Mobile Phase

“…The surface of PGC is composed of flat sheets of hexagonally arranged carbon atoms, as in a very large polynuclear aromatic molecule with no chemically bonded phase (Thermo Electron Corporation, , ). In recent years, PGC column has been widely applied in the analysis of nucleotides (Crauste et al, ; Wang et al, ), ionic compounds (Saitoh, Soeta, Minamisawa, & Shibukawa, ), saccharides (Balogh, Jankovics, & Beni, ; Ji, Hu, Zhang, Wang, & Liu, ), isomers (De Matteis et al, ; Svetlov, Yashkina, Popov, & Yashkin, ), biological samples (Chen et al, ; Szoboszlai et al, ; Virus, Luzyanin, Ivanov, & Kubatiev, ), medicine, and their chiral compounds (Barrow, Castel, Sykes, Myers, & Ritchie, ; Chirita, Finaru, & Elfakir, ; Kalogria & Koupparis, ; Lecoeur‐Lorin, Delépée, Adamczyk, & Morin, ), and so on. However, the use of PGC columns to characterize TAG from edible oils has not been published pervasively.…”