A mussel tissue certified reference material for multiple phycotoxins. Part 1: design and preparation

• Published in: Analytical and bioanalytical chemistry 2011-05, Vol.400 (3), p.821-833
• Main Authors: McCarron, Pearse, Emteborg, Håkan, Nulty, Cíara, Rundberget, Thomas, Loader, Jared I., Teipel, Katharina, Miles, Christopher O., Quilliam, Michael A., Hess, Philipp
• Format: Article
• Language: English
• Subjects: Analysis; Analytical Chemistry; Animals; Biochemistry; Bivalvia - chemistry; Characterization and Evaluation of Materials; Chemistry; Chemistry and Materials Science; Chromatographic methods and physical methods associated with chromatography; Chromatography, Liquid - standards; Customer relationship management software; Exact sciences and technology; Extraction; Food Science; Freeze Drying; General, instrumentation; Laboratory Medicine; Life Sciences; Liquid chromatography; Marine; Marine toxins; Marine Toxins - analysis; Mass spectrometry; Mass Spectrometry - standards; Materials handling; Mathematical analysis; Moisture content; Monitoring/Environmental Analysis; Original Paper; Other chromatographic methods; Reference materials; Reference Standards; Shellfish; Spectrometric and optical methods; Toxins
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-011-4786-9

The development of multi-analyte methods for lipophilic shellfish toxins based on liquid chromatography–mass spectrometry permits rapid screening and analysis of samples for a wide variety of toxins in a single run. Validated methods and appropriate certified reference materials (CRMs) are required to ensure accuracy of results. CRMs are essential for accurate instrument calibration, for assessing the complete analytical method from sample extraction to data analysis and for verifying trueness. However, CRMs have hitherto only been available for single toxin groups. Production of a CRM containing six major toxin groups was achieved through an international collaboration. Preparation of this material, CRM-FDMT1, drew on information from earlier studies as well as improved methods for isolation of toxins, handling bulk tissues and production of reference materials. Previous investigations of stabilisation techniques indicated freeze-drying to be a suitable procedure for preparation of shellfish toxin reference materials and applicable to a wide range of toxins. CRM-FDMT1 was initially prepared as a bulk wet tissue homogenate containing domoic acid, okadaic acid, dinophysistoxins, azaspiracids, pectenotoxin-2, yessotoxin and 13-desmethylspirolide C. The homogenate was then freeze-dried, milled and bottled in aliquots suitable for distribution and analysis. The moisture content and particle size distribution were measured, and determined to be appropriate. A preliminary toxin analysis of the final material showed a comprehensive toxin profile. Figure Bottling of CRM-FDMT1