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Articles

Quantitative determination of paralytic shellfish toxins in cultured toxic algae by LC-MS/MS

, , , , &
Pages 1351-1357 | Received 30 Apr 2012, Accepted 03 Apr 2013, Published online: 02 Jun 2013
 

Abstract

We developed a sample preparation and LC-MS/MS method for the determination of saxitoxins in toxic algae. Paralytic shellfish toxins (PSTs) were successfully separated by gradient elution on an amide column with the hydrophilic interaction mode and quantified with multiple reaction monitoring (MRM) detection in the positive ion mode. This method showed good performance in the summed LODs and LOQs for all 12 toxins, 25 and 84 nM, respectively. Next, extracts of cultured strains of a toxic dinoflagellate Alexandrium tamarense and a freshwater cyanobacteria Anabaena circinalis were treated in a short column of basic alumina and the toxic fractions were analysed by our LC-MS/MS method and by HPLC with fluorescence detection. Comparison of the results obtained by the two methods demonstrated that approximately equivalent results were obtained for both the dinoflagellate and the cyanobacteria. In addition, the retention time of the toxins showed acceptable shifts. Therefore, the clean-up of the toxic algal extracts by using the basic alumina column controlled unwanted chromatographic behaviour and variable ionisation efficiency during MS detection. LC-MS/MS for saxitoxins has great potential as a rapid analytical method for determining all primary saxitoxins in cultured algae.

Acknowledgement

We thank Dr. Blackburn at CSIRO Hobart, Australia, for permitting us to use the freshwater cyanobacteria Anabaena circinalis, TA04 strain.

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