RT Journal Article
T1 Speciation of manganese binding to biomolecules in pine nuts (Pinus pinea) by two-dimensional liquid chromatography coupled to ultraviolet and inductively coupled plasma mass spectrometry detectors followed by identification by electrospray ionization mass spectrometry
A1 Arias Borrego, Ana
A1 García Barrera, Tamara
A1 Gómez Ariza, José Luis
AB Advances in analytical methodology for speciation of manganese in pine nuts are presented in thiswork. The approach is based on the use of orthogonal chromatographic systems, namely sizeexclusionchromatography (SEC) of the extracts and strong anion exchange (IEC) of the fractionscollected by the first column. In both columns, manganese elution is first monitored by a quadrupoleinductively coupled plasma mass spectrometry (ICP-MS) instrument equipped with an octopolereaction cell and an ultraviolet (UV) detector. SEC is performed by using two columns coveringthe molecular weight range from <10 to 70 kDa that allows an initial screening of the molecularweight of theMnspecies. The higher resolution capability of the low molecular weight range columnis the reason to use the latter for further experiments. The fraction from SEC-ICP-MS in which Mn ispresent at highest concentration is submitted to IEC-ICP-MS allowing Mn-citrate and MnCl2identification by retention time matching with standards. The concentration of these species isestimated to be 75 and 125mgkgS1 (as Mn), respectively, in the pine nuts samples and the presence ofMn-citrate is confirmed by nanoelectrospray ionization quadrupole time-of-flight mass spectrometry(nESI-QqTOF-MS). In the same fraction, a third Mn-containing peak is detected in the IEC-UV-ICPMSchromatogram. This peak corresponds to a protein containing Mn that was later submitted to atryptic digestion and analyzed by nESI-QqTOF. The MS/MS data of a doubly charged peptide areused to obtain the sequence of the protein with the Mascot search engine. The peak turned out to beisocitrate dehydrogenase, a protein commonly associated with Mn
SN 0951-4198
SN 1097-0231 (electrónico)
YR 2008
FD 2008
LK https://hdl.handle.net/10272/22967
UL https://hdl.handle.net/10272/22967
LA eng
NO Arias‐Borrego, A., García‐Barrera, T., & Gómez‐Ariza, J. L. (2008). Speciation of manganese binding to biomolecules in pine nuts (Pinus pinea) by two‐dimensional liquid chromatography coupled to ultraviolet and inductively coupled plasma mass spectrometry detectors followed by identification by electrospray ionization mass spectrometry. In Rapid Communications in Mass Spectrometry (Vol. 22, Issue 19, pp. 3053–3060). Wiley. https://doi.org/10.1002/rcm.3704
NO The authors are indebted to the ‘Ministerio de Ciencia y Tecnología (MCyT)’ for Grant No. REN2002-04366-C02-02.
DS Repositorio Institucional de la Universidad de Huelva
RD 30 may 2026