title: Development of reference materials for paralytic shellfish poisoning toxins.
abstract: A project was undertaken to develop mussel reference materials that were certified for their mass fractions of saxitoxin and decarbamoyl-saxitoxin. Fifteen laboratories from various European countries participated. Three of these had major responsibility for substantial parts of the work and overall coordination of the project. The project involved 4 main activities: (1) procurement and characterization of calibrants; (2) improvement of analytical methodology; (3) preparation of reference materials, including homogeneity and stability studies; (4) 2 interlaboratory studies and a certification exercise. The joint activities resulted in 3 homogeneous and stable reference materials: 2 lyophilized mussel materials with and without naturally incurred paralytic shellfish poisoning (PSP) toxins, and a saxitoxin enrichment solution. The reference materials were certified with respect to their saxitoxin and decarbamoyl-saxitoxin content. The lyophilized mussel material with PSP toxins (CRM 542) contained <0.07 mg saxitoxin x 2HCl/kg and 1.59 +/- 0.20 mg decarbamoyl-saxitoxin x 2HCl/kg. The lyophilized mussel material without PSP toxins (CRM 543) contained <0.07 mg saxitoxin x 2HCl/kg and <0.04 mg decarbamoyl-saxitoxin x 2HCl/kg. The certified value of the saxitoxin mass fraction in the saxitoxin enrichment solution (CRM 663) was 9.8 +/- 1.2 microg/g.
authors.affiliation: National Institute of Public Health and the Environment, Laboratory for Residue Analysis, Bilthoven, The Netherlands.
authors.forename: H P
authors.initials: HP
authors.lastname: van Egmond
authors.forename: A
authors.initials: A
authors.lastname: Mouriño
authors.forename: P A
authors.initials: PA
authors.lastname: Burdaspal
authors.forename: A
authors.initials: A
authors.lastname: Boenke
mesh_terms: D000818:Animals; D049872:Bivalvia / Q000737:chemistry*; D002138:Calibration; D002568:Certification; D005612:Freeze Drying; D010243:Paralysis / Q000139:chemically induced*; D012015:Reference Standards; D015203:Reproducibility of Results; D012530:Saxitoxin / Q000031:analogs & derivatives / Q000032:analysis*; D012758:Shellfish / Q000032:analysis*
chemical_list: D012530:Saxitoxin