A mussel tissue certified reference material for multiple phycotoxins. Part 4: certification

Abstract

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Fatty acid esters of azaspiracids identified in mussels (Mytilus edulis) using liquid chromatography-high resolution mass spectrometry

“…3- O -palmitoylAZA4 and 3- O -oleoylAZA4 (the 16:0 and 18:1 esters, respectively) were detected in all samples evaluated. CRM-FDMT1 and CRM-AZA-Mus ( McCarron et al, 2015 , 2017 ) contained trace levels of additional AZA4 fatty acid esters ( Table S2 ), primarily those that had a peak area >10% relative to 3- O -palmitoylAZA4 in the Bruckless sample ( Table 1 ). The content of 3- O -palmitoylAZA4 was estimated in the tissue extracts based on the peak areas of its [M+H] + ion in full scan mode relative to that of AZA4 in the certified tissue of CRM-FDMT1 assuming the same molar response factor, and is summarized in Table 2 .…”

Differential Mobility-Mass Spectrometry Double Spike Isotope Dilution Study of Release of β-Methylaminoalanine and Proteinogenic Amino Acids during Biological Sample Hydrolysis

“…Muscle tissue from the legs and tail were homogenized in a blender, freeze dried, and ground by mortar and pestle. A mussel ( Mytilus edulis ) tissue RM certified for several marine algal biotoxins (CRM-FDMT) was acquired from the National Research Council Canada (Halifax, Canada) 41 – 44 . A recently developed pilot scale cyanobacterial RM that has been extensively characterized for a wide range of cyanotoxins was used as a negative control for BMAA 45 .…”

What is novel about certified reference materials?

“…A series of papers describing development of a new freezedried mussel tissue material (CRM-FDMT1) for multiple phycotoxins was published by McCarron and coworkers [16][17][18][19]. The papers described the various aspects of CRM development including design and preparation [17]; LC-MS/ MS, extraction, and quantification approaches [18]; homogeneity and stability [16] and certification [19].…”

“…The papers described the various aspects of CRM development including design and preparation [17]; LC-MS/ MS, extraction, and quantification approaches [18]; homogeneity and stability [16] and certification [19]. Prior to the development of CRM-FDMT1, mussel tissue CRMs were available only for single toxin groups.…”

“…CRM-FDMT1 was prepared as a mixture of five batches of mussels from different locations and contaminated with six different toxin groups, i.e., domoic acid, DSPs, azapiracids, pectenotoxins, yessotoxinsm, and spirolides. For the certification measurements, LC-MS/MS methods, which were optimized for each toxin group, were employed following exhaustive extraction procedures [19]. To compensate for LC-MS/MS matrix effects, a variety of quantification approaches were used including standard addition, dilution, or matrix-matched calibration.…”