Quantitative Determination of Paralytic Shellfish Poisoning Toxins in Shellfish Using Prechromatographic Oxidation and Liquid Chromatography with Fluorescence Detection: Collaborative Study

Abstract

A collaborative study was conducted for the determination of paralytic shellfish poisoning (PSP) toxins in shellfish. The method used liquid chromatography with fluorescence detection after prechromatographic oxidation of the toxins with hydrogen peroxide and periodate. The PSP toxins studied were saxitoxin (STX), neosaxitoxin (NEO), gonyautoxins 2 and 3 (GTX2,3; together), gonyautoxins 1 and 4 (GTX1,4; together), decarbamoyl saxitoxin (dcSTX), B-1 (GTX5), C-1 and C-2 (C1,2; together), and C-3 and C-4 (C3,4; together). B-2 (GTX6) toxin was also included, but for qualitative identification only. Mussels, both blank and naturally contaminated, were mixed and homogenized to provide a variety of PSP toxin mixtures and concentration levels. The same procedure was followed with clams, oysters, and scallops. Twenty-one test samples in total were sent to 21 collaborators who agreed to participate in the study. Results were obtained from 18 laboratories representing 14 different countries. It is recommended that the method be adopted First Action by AOAC INTERNATIONAL.

Warm temperature acclimation impacts metabolism of paralytic shellfish toxins from Alexandrium minutum in commercial oysters

“…The PST content was measured in 300 individual oysters (n = 9 oysters per toxic treatment and n = 30 nontoxic control oysters), according to Lawrence et al (2005) and Harwood et al (2013). Briefly, homogenised (Omni Tissue Homogeniser, Omni International, USA) oyster tissue was vortexed with 3 mL of 1% acetic acid solution.…”

Prevalence of paralytic shellfish poison-producing Planktothrix agardhii and Cylindrospermopsis raciborskii in a Brazilian semi-arid reservoir

“…However, one peak was observed at 2.86 min in the sample oxidized with peroxide ( Figure 5b). The detected peak might represent dcGTX2 or dcGTX3 based on the peak detection sequence proposed by Lawrence et al (2005).…”

“…The sample was then subjected to a pre-purification step by solid phase extraction (SPE) on C18 cartridges (Supelco). Separation of the different PSPs potentially present was performed by SPE with a 3mL carboxylic acid cartridges (Supelco), according to Lawrence et al (2005).…”

“…From 13 to 15 min, flow returned to 100% of A. The above methodology was adapted from Lawrence et al (2005).…”

Marine biotoxins in shellfish – Saxitoxin group

“…The method was described by Lawrence and Menard (1991) and was evaluated in 2002 in an international collaborative study involving 18 laboratories (Lawrence et al, 2004(Lawrence et al, , 2005. It was successfully validated for the toxins GTX1 and GTX4 together, GTX2 and GTX3 together, C1 and C2 together, C3 and C4 together, NeoSTX, STX, dcSTX and GTX5.…”