A convenient HPLC method for detection of okadaic acid analogs as 9-anthrylmethyl esters with automated sample cleanup by column switching.
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.
Hajime
H
Uchida
Ryuichi
R
Watanabe
Ryoji
R
Matsushima
Naoyuki
N
Uchida
Hiroshi
H
Nagai
Michiya
M
Kamio
Masakazu
M
Murata
Takeshi
T
Yasumoto
Toshiyuki
T
Suzuki
D000818:Animals; D000873:Anthracenes / Q000737:chemistry; D001331:Automation; D049872:Bivalvia / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004952:Esters / Q000737:chemistry*; D059022:Food Safety; D008387:Marine Toxins / Q000737:chemistry; D015394:Molecular Structure; D019319:Okadaic Acid / Q000031:analogs & derivatives* / Q000737:chemistry*; D011714:Pyrans / Q000737:chemistry; D053719:Tandem Mass Spectrometry
D000873:Anthracenes; D004952:Esters; D008387:Marine Toxins; D011714:Pyrans; D019319:Okadaic Acid; C051904:dinophysistoxin 1