A mussel tissue certified reference material for multiple phycotoxins. Part 3: homogeneity and stability

Abstract

A candidate certified reference material (CRM) for multiple shellfish toxins (domoic acid, okadaic acid and dinophysistoxins, pectenotoxins, yessotoxin, azaspiracids and spirolides) has been prepared as a freeze-dried powder from mussel tissues (Mytilus edulis). Along with the certified values, the most important characteristics for a reference material to be fit-for-purpose are homogeneity and stability. Acceptable between-bottle homogeneity was found for this CRM. Within-bottle homogeneity was assessed using domoic acid, and it was shown that repeated subsampling of the CRM can be performed precisely down to 0.35 g. Both short- and long-term stability studies carried out under isochronous conditions demonstrated excellent stability of the various toxins present in the material. While degradation of some analytes was observed at +60°C in short-term studies, it was determined that shipping at ambient temperature is adequate. No instability was detected in long-term stability studies, and it was shown that the material can be held at +18°C safely for up to 1 year. To guarantee stability of the CRM over its lifetime the stock will be maintained at -20°C. The results of the homogeneity and stability testing show that CRM-FDMT1 is appropriate for its intended use in quality assurance and quality control of shellfish toxin analysis methods.

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

“…LC-MS is the only detection and measurement technique offering sufficient sensitivity and precision for most of the target analytes in CRM-FDMT1. Although a multi-toxin LC-MS method was developed earlier in this project [16] for use in homogeneity and stability testing [17], the extraction and analysis methods needed to be further refined for specific toxin groups in order to achieve the level of extraction efficiency favorable for certification. Toxinspecific LSE and MSPD procedures were optimized to exhaustively extract individual toxin groups in CRM-FDMT1.…”

“…material contains notable levels of analytes from six major groups of shellfish toxins, including domoic acid (DA), azaspiracids (AZAs), okadaic acid (OA) and dinophysistoxins (DTXs), pectenotoxins (PTXs), yessotoxins (YTXs), and spirolides (SPXs). Development of extraction and LC-MS methods [16] preceded a comprehensive assessment of the homogeneity and stability of CRM-FDMT1 [17]. Homogeneity was found to be excellent across the entire production series, while stability studies showed no degradation at temperatures as high as +18°C over 1 y.…”

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.…”

PAH Analytics in New Polish Reference Material

“…In such kinds of analysis, it is particularly important to provide the adequate quality of the process and obtain reliable results (quality assurance QA and quality control QC) [1][2][3]. Therefore, the task becomes more difficult when the concentration of a substance tested decreases and the complexity of the matrices composition increases [4][5][6]. The quality of our life depends on the reliability of the measurement results (physical as well chemical quantities), which often influence our decisions.…”