title: Rapid determination of domoic acid in serum and urine by liquid chromatography-electrospray tandem mass spectrometry.
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 microg/g method detection limit (MDL) and at the 0.05 microg/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.
authors.affiliation: Toxicology Laboratory, California Animal Health and Food Safety Laboratory System, University of California, Davis, California 95616, USA. ertor@ucdavis.edu
authors.forename: Elizabeth R
authors.initials: ER
authors.lastname: Tor
authors.forename: Birgit
authors.initials: B
authors.lastname: Puschner
authors.forename: William E
authors.initials: WE
authors.lastname: Whitehead
mesh_terms: D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D007608:Kainic Acid / Q000031:analogs & derivatives* / Q000097:blood* / Q000652:urine*; D008387:Marine Toxins / Q000097:blood* / Q000652:urine*; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization
chemical_list: D008387:Marine Toxins; C012301:domoic acid; D007608:Kainic Acid