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Domoic Acid in Seafood Samples
      Domoic Acid (DA) From Seafood Without Derivatization

charts
A – Extract from mussels (low concentration)
B – Extract from mussels (high concentration)
C – Fish extract
D – Plankton high and low concentration of domoic acid
E – Standard of domoic acid
F – 5 Overlaid injections of plankton extract sample

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Notes: Data was presented at the American Society of Pharmacognosy Annual Meeting and Exhibition, July 30 – August 3, 2011, San Diego, California.
Method Conditions



Column Cogent Diamond Hydride™, 4µm, 100A
Catalog No. 70000-15P-2
Dimensions 2.1 x 150 mm
Solvents
A:50% MeOH/ 50% DI H2O/ 0.1% formic acid
B:Acetonitrile/ 0.1% formic acid
Gradient
time (min.) %B time (min.) %B
0 95 8 30
7 30 10 95
Post Time 5 min
Injection Vol. 1 microL
Flow rate 0.4 mL/min.
Detection ESI - POS - Agilent 6210 MSD TOF MS
Samples Samples from Dr. R.Kudela, Univ. of Calif., Santa Cruz,
Dept. of Marine Sciences. Samples were injected as received.
Peak Domoic acid 312.1442 m/z (M+H)+
t0 0.9 min

Discussion

Several seafood and plankton samples were tested for domoic acid (DA) which, as a highly polar compound, is poorly retained on most reversed phase columns. This developed method based on HPLC and MS detection does not require derivatization of DA. The concentration of this potent toxin varied quite substantially between the samples (from 40 ng/mL in plankton to 3700 ng/mL in mussels). Despite different sample matrices, it was possible to detect and analyze domoic acid in a wide range of concentrations.

The results were very repeatable (see 5 overlaid injections in Figure F). The detection limit depends on the instrument used. The method can be used by regulatory agencies responsible for monitoring the occurrence of toxins such as the analysis of domoic acid in seafood samples.




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