title: A fast and simple solid phase microextraction coupled with gas chromatography-triple quadrupole mass spectrometry method for the assay of urinary markers of glutaric acidemias.
abstract: The analysis of characteristic urinary acidic markers such as glutaric, 3-hydroxyglutaric, 2-hydroxyglutaric, adipic, suberic, sebacic, ethylmalonic, 3-hydroxyisovaleric and isobutyric acid constitutes the recommended follow-up testing procedure for glutaric acidemia type 1 (GA-1) and type 2 (GA-2). The goal of the work herein presented is the development of a fast and simple method for the quantification of these biomarkers in human urine. The proposed analytical approach is based on the use of solid phase microextraction (SPME) combined with gas chromatography-triple quadrupole mass spectrometry (GC-QqQ-MS) afterward a rapid derivatization of acidic moieties by propyl chloroformate, propanol and pyridine. Trueness and precision of the proposed protocol, tested at 5, 30 and 80mgl-1, provided satisfactory values: recoveries were in the range between 72% and 116% and the relative standard deviations (RSD%) were between 0.9% and 18% (except for isobutyric acid at 5mgl-1). The LOD values achieved by the proposed method ranged between 1.0 and 473μgl-1.
authors.affiliation: Dipartimento di Chimica e Tecnologie Chimiche, Università della Calabria, Via P. Bucci Cubo 12/C, I-87030 Arcavacata di Rende (CS), Italy.
authors.forename: Attilio
authors.initials: A
authors.lastname: Naccarato
authors.affiliation: Dipartimento di Chimica e Tecnologie Chimiche, Università della Calabria, Via P. Bucci Cubo 12/C, I-87030 Arcavacata di Rende (CS), Italy.
authors.forename: Emanuela
authors.initials: E
authors.lastname: Gionfriddo
authors.affiliation: Dipartimento di Chimica e Tecnologie Chimiche, Università della Calabria, Via P. Bucci Cubo 12/C, I-87030 Arcavacata di Rende (CS), Italy.
authors.forename: Rosangela
authors.initials: R
authors.lastname: Elliani
authors.affiliation: Dipartimento di Chimica e Tecnologie Chimiche, Università della Calabria, Via P. Bucci Cubo 12/C, I-87030 Arcavacata di Rende (CS), Italy.
authors.forename: Giovanni
authors.initials: G
authors.lastname: Sindona
authors.affiliation: Dipartimento di Chimica e Tecnologie Chimiche, Università della Calabria, Via P. Bucci Cubo 12/C, I-87030 Arcavacata di Rende (CS), Italy. Electronic address: a.tagarelli@unical.it.
authors.forename: Antonio
authors.initials: A
authors.lastname: Tagarelli
keywords: Alkyl chloroformate; Gas chromatography; Glutaric acidemia; Organic acidemia; Solid phase microextraction; Urine