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Title of Journal: Anal Bioanal Chem

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Abbravation: Analytical and Bioanalytical Chemistry

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Springer-Verlag

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10.1007/430_2013_105

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1618-2650

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Development and validation of a rapid method for m

Authors: Lucía GeisAsteggiante Steven J Lehotay Laurie L Fortis George Paoli Chandi Wijey Horacio Heinzen
Publish Date: 2011/09/01
Volume: 401, Issue: 8, Pages: 2617-2630
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Abstract

Microcystins MCs are the most common cyanotoxins found worldwide in freshwater brackish and marine environments The rapid and accurate analysis of MCs and nodularin NodR in fish tissue is important for determining occurrence following trends and monitoring exposure for risk assessment and other purposes The aim of this study was to develop a streamlined and reliable sample preparation method for eight MCs MCRR MCYR MCLR MCWR MCLA MCLY MCLW and MCLF and NodR in fish and conduct a validation of the new method using liquid chromatography–tandem mass spectrometry LCMS/MS for analysis and compare the results with a commercial enzymelinked immunosorbent assay ELISA kit Different sample preparation methods were compared and a simple extraction protocol with acidified acetonitrile/water 31 followed by hexane partitioning cleanup was found to be most effective Thorough validation of the final method was conducted and 90–115 recoveries were achieved for all analytes except for MCRR which gave 130 average recovery isotopically labeled internal standards were unavailable to correct for possible biases The use of electrospray ionization in the negative mode gave few interferences and minimal matrix effects in the LCMS/MS analysis overall Precision was typically 10–20 RSD among multiple days in experiments detection limits were 10 ng/g in the fish tissue catfish basa and swai filets and no falsepositives or falsenegatives occurred in blind analyses of many spiked samples The ELISA was unable to distinguish between MCs but was found to correctly assess the presence or absence of MCs and NodR in the blindfortified fish tissues The capability of these approaches to measure covalently bound MCs was not assessedWe thank Jennifer Cassidy and Kathleen Rajkowski for providing the different fish samples Alan Lightfield for his support in LCMS/MS usage and Fernando Rubio of Abraxis for consultation about microcystins and ELISA This research was funded in part by the USDA Food Safety Inspection Service ARS agreement number 6019359031 and the US–Israel Binational Agricultural Research and Development Fund number US427309

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