title: A gas chromatography-mass spectrometry multi-target method for the simultaneous analysis of three classes of metabolites in marine organisms.
abstract: In this work a fast and simple multi-target gas chromatography-mass spectrometry (GC-MS) method for the simultaneous detection and absolute quantification of amino acids, fatty acids, sterols and lupanes in marine organisms is proposed. The methodology was applied to the characterization of the echinoderm Marthasterias glacialis Linnaeus spiny sea star extracts. The main factors influencing the extraction of target compounds were evaluated by using different extraction procedures, solvent systems and temperature conditions and a comparison with a reference technique was performed. The most suitable procedure, capable of successfully extract the three classes of target compounds, was ethanol as solvent at 40°C under magnetic stirring. Good analytical parameters were obtained since calibrations curves for the 40 compounds under analysis (15 amino acids, 16 fatty acids, 6 sterols and 3 lupanes) showed regression coefficients (r(2)) ranging from 0.9844 to 0.9978, with low RSD (from 0.00 to 9.45%), and detection limits varying from 0.03 to 15.40 μg/L. The RSD values for intra- and interday variations studies were also good (RSD<13.5%, for both) and recoveries were higher than 92%. Variation in samples from different harvests and origins and their chemical composition during the year is reported. The fact that no previous treatment of samples is required can make this a useful technique for metabolite profiling in marine organisms, among others, both in biomedical and nutritional studies. Moreover, due to the fast and robust character of the proposed method it seems to be suitable for the implementation as routine analysis.
authors.affiliation: REQUIMTE/Laboratório de Farmacognosia, Departamento de Química, Faculdade de Farmácia, Universidade do Porto, Rua de Jorge Viterbo Ferreira n.º 228, 4050-313 Porto, Portugal.
authors.forename: David M
authors.initials: DM
authors.lastname: Pereira
authors.forename: Juliana
authors.initials: J
authors.lastname: Vinholes
authors.forename: Paula Guedes
authors.initials: PG
authors.lastname: de Pinho
authors.forename: Patrícia
authors.initials: P
authors.lastname: Valentão
authors.forename: Teresa
authors.initials: T
authors.lastname: Mouga
authors.forename: Natércia
authors.initials: N
authors.lastname: Teixeira
authors.forename: Paula B
authors.initials: PB
authors.lastname: Andrade
mesh_terms: D000596:Amino Acids / Q000302:isolation & purification / Q000378:metabolism; D000818:Animals; D059001:Aquatic Organisms / Q000378:metabolism*; D004447:Echinodermata / Q000378:metabolism; D005227:Fatty Acids / Q000302:isolation & purification / Q000378:metabolism; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D057230:Limit of Detection; D013261:Sterols / Q000302:isolation & purification / Q000378:metabolism; D013997:Time Factors; D014315:Triterpenes / Q000302:isolation & purification / Q000378:metabolism; D053978:Pentacyclic Triterpenes
chemical_list: D000596:Amino Acids; D005227:Fatty Acids; D013261:Sterols; D014315:Triterpenes; C480546:lupane; D053978:Pentacyclic Triterpenes