TY - JOUR
T1 - LC-ESI-Q-TOF-MS for faster and accurate determination of microcystins and nodularins in serum
AU - Neffling, Milla Riina
AU - Spoof, Lisa
AU - Quilliam, Michael
AU - Meriluoto, Jussi
N1 - Funding Information:
ISB graduate school, Stiftelsens för Åbo Akademi forskningsinstitut, Harry Elvings Legat, Systems Biology Research program, Academy of Finland (decision number 108947), Medicinska understödsföreningen Liv och Hälsa and The Otto A. Malm foundation are thanked for their financial support.
Copyright:
Copyright 2011 Elsevier B.V., All rights reserved.
PY - 2010/9
Y1 - 2010/9
N2 - Microcystins (MC) and nodularins (Nod) are cyclic peptide hepatotoxins and tumour promoters produced by cyanobacteria. This study deals with liquid chromatography-mass spectrometry (LC-MS) analyses of 9 major cyanobacterial peptide toxins, starting with a comparison of six small particle size reversed-phase HPLC columns, from which one, Phenomenex Synergi Hydro-RP, was chosen for further chromatography with accurate mass MS studies in a complex biological fluid, serum. The instrumentation used for the serum sample analysis included a Bruker micrO-TOF-Q-MS coupled to an Agilent 1200RR LC system. Total analysis run time per sample was 8.5. min. The Q-TOF-MS instrument was operated on auto MS-MS mode to obtain fragment ions (such as the characteristic fragment m/z 135 from Adda amino acid residue) for toxin identification purposes. Detected mass errors in serum samples were in the range of from 0.3. mDa to 9.1. mDa. The narrow mass window (±20. mDa) for mass chromatograms used in quantitation gave benefits by background noise reduction. We conclude that a LC-ESI-Q-TOF-MS instrumentation is a powerful tool for identification and quantitation of cyanobacterial peptide toxins in a biological matrix.
AB - Microcystins (MC) and nodularins (Nod) are cyclic peptide hepatotoxins and tumour promoters produced by cyanobacteria. This study deals with liquid chromatography-mass spectrometry (LC-MS) analyses of 9 major cyanobacterial peptide toxins, starting with a comparison of six small particle size reversed-phase HPLC columns, from which one, Phenomenex Synergi Hydro-RP, was chosen for further chromatography with accurate mass MS studies in a complex biological fluid, serum. The instrumentation used for the serum sample analysis included a Bruker micrO-TOF-Q-MS coupled to an Agilent 1200RR LC system. Total analysis run time per sample was 8.5. min. The Q-TOF-MS instrument was operated on auto MS-MS mode to obtain fragment ions (such as the characteristic fragment m/z 135 from Adda amino acid residue) for toxin identification purposes. Detected mass errors in serum samples were in the range of from 0.3. mDa to 9.1. mDa. The narrow mass window (±20. mDa) for mass chromatograms used in quantitation gave benefits by background noise reduction. We conclude that a LC-ESI-Q-TOF-MS instrumentation is a powerful tool for identification and quantitation of cyanobacterial peptide toxins in a biological matrix.
KW - Cyclic peptides
KW - LC-ESI-Q-TOF-MS
KW - Microcystins
KW - Serum
KW - Sub-3 micron particle columns
UR - http://www.scopus.com/inward/record.url?scp=77956246434&partnerID=8YFLogxK
U2 - 10.1016/j.jchromb.2010.07.018
DO - 10.1016/j.jchromb.2010.07.018
M3 - Article
C2 - 20724233
AN - SCOPUS:77956246434
SN - 1570-0232
VL - 878
SP - 2433
EP - 2441
JO - Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences
JF - Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences
IS - 26
ER -