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Method Abstract for Post-column Liquid Chromatography 105.1

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The paralytic shellfish toxins are a group of 18 secondary metabolites deposited in bivalve mollusks by dinoflagelates.  Dinoflagelates blooms are seasonal, occuring during warm months.  Since it is unpredictable whether an infestation will occur, the shellfish population should be regularly monitored for toxins.  Ingestion of contaminated shellfish can lead to paralytic shellfish poisoning; a life-threatening illness.

 

METHOD

Analytical Conditions

COLUMN:

Reversed-phase column for PST analysis,
C8, 4.6 x 150 mm, Catalog No. 0846150

TEMPERATURE:

40 °C

FLOW RATE:

0.8 mL/min

MOBILE PHASE:

A. For C1–C4 toxins:

 

Tetrabutylanmmonium phosphate (1 mM) adjusted to pH 5.8 with acetic acid

B. For GTX-1 to GTX-6, dcGTX2, and dcGTX3:

  Sodium 1-heptanesulfonate (2 mM)
in 10 mM Ammonium phosphate, pH 7.1
C. For STX, neoSTX, and dcSTX:
  Sodium 1-heptanesulfonate (2 mM) in 10 mM Ammonium phosphate, pH 7.1 :
Acetonitrile (2 : 1)

Post-column Conditions

POST-COLUMN  SYSTEM:

Vector PCX or Piinnacle PCX

REAGENT 1: Periodic acid (7 mM) in 50 mM
Potassium Phosphate buffer, pH 9.0
REACTOR 1: 75 °C, 2.0 mL
REAGENT 2: 0.5 M Acetic Acid
REACTOR 2: ambient, 0.1 mL
FLOW RATE: 0.4 mL/min each
DETECTION: Fluorometer
ex: 330 nm
em: 390 nm

REFERENCES

1.  Y. Oshima, K Sugino, T. Yasumoto
“Latest Advances in HPLC Analysis of Paralytic Shellfish
Toxins in Bioactiva Molecules” 10, (1989) 319–326

2.  J. J. Sullivan, M.M. Wekell, and L. L. Kentala,
J. Food Sci. 50(1) (1985) 26–29.

3.  Y. Oshima, JOAC, INTL. 78(2) (1995)

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