Determination of α-amanitin in serum and liver by multistage linear ion trap mass spectrometry

Michael S. Filigenzi, Robert H Poppenga, Asheesh K. Tiwary, Birgit Puschner

Research output: Contribution to journalArticle

43 Scopus citations

Abstract

This paper describes a rapid LC-MS/MS/MS method for the analysis of α-amanitin in serum and liver. Serum was initially prepared by precipitation of proteins with acetonitrile and subsequent removal of acetonitrile with methylene chloride. Liver was prepared by homogenization with aqueous acetonitrile and subsequent removal of acetonitrile using methylene chloride. For both matrices, the aqueous phase was then extracted using mixed-mode C18/cation exchange SPE cartridges and analyzed on a linear ion trap LC-MS system. Standards were prepared in extracts of control matrix. Seven replicate fortifications of serum at 0.001 μg/g (1 ng/g) of α-amanitin gave a mean recovery of 95% with 8.8% CV (relative standard deviation) and a calculated method detection limit of 0.26 ng/g. Seven replicates of control liver fortified at 1 ng/g gave a mean recovery of 98% with 17% CV and a calculated method detection limit of 0.50 ng/g. This is the first report of a positive mass spectrometric identification and quantitation of α-amanitin in serum and liver from suspect human and animal intoxications.

Original languageEnglish (US)
Pages (from-to)2784-2790
Number of pages7
JournalJournal of Agricultural and Food Chemistry
Volume55
Issue number8
DOIs
StatePublished - Apr 18 2007

Keywords

  • Amanitin
  • Ion trap
  • LC-MS
  • Liquid chromatography
  • Mass spectrometry

ASJC Scopus subject areas

  • Agricultural and Biological Sciences (miscellaneous)
  • Food Science
  • Chemistry (miscellaneous)

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