Rapid determination of domoic acid in serum and urine by liquid chromatography-electrospray tandem mass spectrometry

Elizabeth R. Tor, Birgit Puschner, William E. Whitehead

Research output: Contribution to journalArticle

20 Citations (Scopus)

Abstract

A rapid, selective, and sensitive LC-MS/MS method was developed for the quantitative determination of domoic acid in serum and urine samples. Samples were prepared for analysis using an Oasis HLB SPE column. Determination was by a reversed phase HPLC using a mixture of methanol, acetonitrile, and water containing 1% acetic acid and an electrospray ionization (ESI) ion-trap mass spectrometer (Finnigan LCQ). The method was validated by analyzing five replicates each of negative control bovine serum or urine fortified with domoic acid at the 0.005 μg/g method detection limit (MDL) and at the 0.05 μg/g level. Recoveries ranged from 90 to 95% for fortifications at the MDL and from 92 to 98% for fortifications 10 times higher than the MDL. The diagnostic utility of the method was tested by analyzing samples from live animals showing clinical signs suggestive of domoic acid poisoning submitted to the veterinary toxicology laboratory.

Original languageEnglish (US)
Pages (from-to)1791-1796
Number of pages6
JournalJournal of Agricultural and Food Chemistry
Volume51
Issue number7
DOIs
StatePublished - Mar 26 2003

Fingerprint

domoic acid
Liquid chromatography
Tandem Mass Spectrometry
Liquid Chromatography
liquid chromatography
Mass spectrometry
urine
Urine
Serum
Limit of Detection
Electrospray ionization
detection limit
Mass spectrometers
Acetic Acid
Methanol
Animals
methodology
Ions
Recovery
Water

Keywords

  • Domoic acid
  • HPLC
  • LC/MS
  • Mass spectrometry
  • Serum
  • Urine

ASJC Scopus subject areas

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

Cite this

Rapid determination of domoic acid in serum and urine by liquid chromatography-electrospray tandem mass spectrometry. / Tor, Elizabeth R.; Puschner, Birgit; Whitehead, William E.

In: Journal of Agricultural and Food Chemistry, Vol. 51, No. 7, 26.03.2003, p. 1791-1796.

Research output: Contribution to journalArticle

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N2 - A rapid, selective, and sensitive LC-MS/MS method was developed for the quantitative determination of domoic acid in serum and urine samples. Samples were prepared for analysis using an Oasis HLB SPE column. Determination was by a reversed phase HPLC using a mixture of methanol, acetonitrile, and water containing 1% acetic acid and an electrospray ionization (ESI) ion-trap mass spectrometer (Finnigan LCQ). The method was validated by analyzing five replicates each of negative control bovine serum or urine fortified with domoic acid at the 0.005 μg/g method detection limit (MDL) and at the 0.05 μg/g level. Recoveries ranged from 90 to 95% for fortifications at the MDL and from 92 to 98% for fortifications 10 times higher than the MDL. The diagnostic utility of the method was tested by analyzing samples from live animals showing clinical signs suggestive of domoic acid poisoning submitted to the veterinary toxicology laboratory.

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