LC-UV and LC-MS methods for the determination of domoic acid

Abstract

Under European legislation, domoic acid (DA), the main constituent of amnesic shellfish poisoning, is monitored to protect the shellfish consumer. To ensure comparability amongst analytical data, it was deemed necessary to undertake performance assessments of the methods conducted by monitoring laboratories of the United Kingdom and Ireland.In phase I of a two-phase inter-comparison, three laboratories used high-performance liquid chromatography and ultraviolet detection (HPLC-UV). Concentration data for a DA standard solution, a crude extract of whole scallops and a scallop-homogenate fell within internationally accepted limits, demonstrating good agreement for these matrices. Between-laboratory analyses of a scallop gonad showed a higher variation (>16%).In phase II, a second gonad homogenate containing DA one order of magnitude higher in concentration gave results acceptable to internationally set criteria.The efficiency of the strong anion-exchange cartridges used in sample-extract clean-up should be monitored as part of a laboratory quality control system.From a recovery study, it is suggested that recovery correction should also be applied. There was no difference in the quantitation of DA in standard solutions or shellfish using either LC-UV or LC with mass spectrometric (MS) detection, and between-laboratory MS data for a gonad homogenate were also equivalent.Variations of the published method practised by the monitoring laboratories were found not to compromise results, thus demonstrating an acceptable degree of ruggedness, as well as comparability between the participants.

Application of Solid Phase Adsorption Toxin Tracking (SPATT) for field detection of the hydrophilic phycotoxins domoic acid and saxitoxin in coastal California

“…A comparative cost analysis for shellfish and SPATT is supplied in Table 4. Shellfish costs were estimated according to the extraction procedure and materials described in established protocols (Hess et al 2005;Quilliam et al 1995;Quilliam et al 1998). While the overhead costs estimated for both monitoring programs are comparable (~$200 USD), the programs differ in per-sampler cost.…”

“…For regulatory monitoring purposes, however, SPATT alone would not be acceptable since it does not conform to AOAC guidelines (AOAC International (Hess et al 2005;Quilliam et al 1995;Quilliam et al 1998). All costs are in 2010 USD ($).…”

Variation in the abundance of Pseudo-nitzschia and domoic acid with surf zone type

“…Analysis of pDA and domoic acid in the Emerita were made following standard techniques. Briefly, filters for pDA were sonicated in 10% methanol and processed using Varian solid phase extraction columns following the method of Wang et al (2012), with quantification on an Agilent 6130 LC/MS as described in Seubert et al (2014) Emerita were processed following the same methods as for shellfish, following Hess et al (2005) with quantification as for pDA.…”

Sensitive determination of domoic acid in shellfish by on-line coupling of weak anion exchange solid-phase extraction and liquid chromatography–diode array detection–tandem mass spectrometry

“…Sample cleanup by strong 0308-8146/$ -see front matter Ó 2011 Elsevier Ltd. All rights reserved. doi:10.1016/j.foodchem.2011.05.004 anion exchange (SAX) solid-phase extraction (SPE) has been demonstrated to reduce matrix interferences from aqueous methanol extracts, achieving much lower LODs while increasing time consumption (Hess et al, 2005;Quilliam, Xie, & Hardstaff, 1995).…”

“…Sensitivity and selectivity are their main advantages, which have made these methods the best choice for unambiguous identification and quantification of DA. Nevertheless, possible matrix effects make necessary an efficient sample cleanup, which usually is carried out by a labour-intensive SAX-SPE procedure (Hess et al, 2001(Hess et al, , 2005.…”