A convenient HPLC method for detection of okadaic acid analogs as 9-anthrylmethyl esters with automated sample cleanup by column switching

J AOAC Int. 2014 Mar-Apr;97(2):391-7. doi: 10.5740/jaoacint.sgeuchida.

Abstract

A convenient HPLC-fluorometric detection (FLD) method for okadaic acid (OA) analogs as 9-anthrylmethyl esters was developed with the addition of column switching to simplify and automate cleanup. Methanol extracts of shellfish were first treated to hydrolyze OA esters and then reacted with 9-anthryldiazomethane (ADAM). ADAM derivatives of OA and dinophysistoxin-1 (DTX1) were subsequently determined by HPLC-FLD following automated column-switching cleanup. The LOD (S/N = 3) and LOQ (S/N = 10) of OA and DTX1 obtained from bivalves fortified with toxin in our method were approximately 2.6 and 8.6 ng/g whole meat, respectively. The recoveries of OA and DTX1 at all fortification levels of bivalve extracts ranged from 90 to 113%, with RSD values of 0.9-9.9%. The new method is applicable to the routine monitoring of OA analogs as an inexpensive and convenient alternative to HPLC/MS.

MeSH terms

  • Animals
  • Anthracenes / chemistry
  • Automation
  • Bivalvia / chemistry
  • Chromatography, High Pressure Liquid / methods*
  • Esters / chemistry*
  • Food Safety
  • Marine Toxins / chemistry
  • Molecular Structure
  • Okadaic Acid / analogs & derivatives*
  • Okadaic Acid / chemistry*
  • Pyrans / chemistry
  • Tandem Mass Spectrometry

Substances

  • Anthracenes
  • Esters
  • Marine Toxins
  • Pyrans
  • Okadaic Acid
  • dinophysistoxin 1