A HILIC-MS/MS method has beendeveloped and validated for quantitation of PSP toxins in 12 species ofmolluscs. The method employs a fast single-step extraction with SPE clean-up.The method has acceptable performance characteristics and compares well withthe regulatory LC-FLD method. Moreover, it provides accurate quantitation, withfaster turnaround and higher throughput, with less reliance on analyst time andeffort. As such it potentially offers an improved monitoring tool forlaboratories wishing to conduct rapid, accurate testing of molluscs for PSPtoxins. However, for such a method to be used for official control testing inthe EU, it must be deemed “Internationally Accepted”.
During 2016, a preliminaryassessment of the method through a small collaborative study was conducted involvingseven laboratories with a range of LC-MS/MS instruments. Six shellfish samples,including oysters, mussels and clams were shipped to each participant and subjectedto the HILIC-MS/MS method. Participants were asked to follow a method protocoldocument and report quantitative results and any issues or comments associatedwith the method.
This presentation will focus onthe results obtained from this preliminary collaborative study. The qualitativeand quantitative comparison of results in will be discussed, including theresults from the analysis of a CRM. The paper will highlight some of the issuesencountered during this assessment, including HILIC columns batches, andmitigation options.
With the results from thisinitial study showing good promise, work will continue to plan and run a fullcollaborative study involving a larger number of participants, during2017-2018.
