4.6 Article

Development and validation of a liquid chromatography-tandem mass spectrometry assay for the simultaneous quantitation of microcystin-RR and its metabolites in fish liver

Journal

JOURNAL OF CHROMATOGRAPHY A
Volume 1217, Issue 9, Pages 1455-1462

Publisher

ELSEVIER
DOI: 10.1016/j.chroma.2009.12.068

Keywords

Microcystin; LC-MS/MS; SPE; Method validation

Funding

  1. Chinese Academy of Sciences [KZCX1-YW-14-6-1]
  2. Ministry of Science and Technology of the People's Republic of China [2007BAC26B02]

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A novel method for identification and quantification of microcystin-RR (MC-RR) and its metabolites (MC-RR-GSH and MC-RR-Cys) in the fish liver was developed and validated. These analytes were simultaneously extracted from fish liver using water containing EDTA with 5% acetic acid, followed by a mixed-mode cation-exchange SPE (Oasis MCX) and subsequently determined by liquid chromatography-electrospray ionization ion trap mass spectrometry (LC-ESI-ITMS). Extraction parameters including volume and pH of eluting solvents, were optimized. Best recoveries were obtained by using 10 mL of 15% ammonia solution in methanol. The mean recoveries at three concentrations (0.2, 1.0, and 5.0 mu g g(-1) dry weight [DW]) for MC-RR, MC-RR-GSH and MC-RR-Cys were 93.6-99%,68.1-73.6% and 90.0-95.2%, respectively. Method detection limit (MDL) were 4, 7 and 5 ng g(-1) DW for MC-RR, MC-RR-GSH and MC-RR-Cys, respectively. Limits of quantification (LOQs) for MC-RR, MC-RR-GSH and MC-RR-Cys were calculated to be 10, 18 and 13 ng g(-1) DW, respectively. Finally, this method was successfully applied to the identification and quantification of MC-RR, MC-RR-GSH and MC-RR-Cys in the liver of bighead carp with acute exposure of MCs. (C) 2009 Elsevier B.V. All rights reserved.

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