Validation azaspiracid

In a series of papers, the group of Volmer [130-132] studied the analysis of azaspiracid biotoxins. Ultrafast and/or high-resolution LC of azaspiracids on monohthic LC columns was evaluated [130]. Chromatograms of five azaspiracids on a 100-mm and a 700-mm monolithic column are shown in Figure 14.11. Fragmentation of azaspiracids in MS-MS on ion-trap and triple-quadrupole instruments was studied as well [131]. The interpretation was confirmed using accurate-mass data from a Q-TOF instrument. Validation of a quantitative method for AZA-1 was also reported [132]. The LOQ was 5 and 50 pg/ml extract using a triple-quadrapole in SRM mode and an ion-trap instrument, respectively. 

P.K.S. Blay, S. Brombacher, D.A. Vohner, Studies on azaspiracid biotoxins. III. Instrumental validation for rapid quantification of AZA-I in complex biological matrices. Rapid Commun. Mass Spectrom., 17 (2003)2153. 

Very recently, Stobo et al. proposed a multiple LC-MS method that allows the detection of YTX together with most of the DSP toxins. The method was set up on a triple quadrupole spectrometer. Chromatographic separation of multiple lipophilic toxins was achieved by using a base deactivated silica C8 column eluted with a 5 mM ammonium acetate-acetonitrile mobile phase under gradient conditions. The method was applied to the analysis of sheUflsh and was validated for the quantitative detection of OA, YTX, PTX-2, and Azaspiracid-1 (AZA-1). 

Liquid chromatography, coupled with mass spectrometry and tandem mass spectrometry (LC-MS/MS), is a universal technique for determining toxins in food. The first multiple reaction monitoring (MRM) method for polyether marine toxins was used for the determination of DSP toxins and this technique has been successfully applied to the simultaneous determination of various groups of polyether toxins in shellfish (Draisci et al., 1998, 1999). MRM involves the selection of a precursor ion and its product ion from CID fragmentations and it is highly selective. For azaspiracids, the first validated LC-MS/MS method was developed for the determination of AZAl... 

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