title: Optimization of Sample Preparation for the Identification and Quantification of Saxitoxin in Proficiency Test Mussel Sample using Liquid Chromatography-Tandem Mass Spectrometry.
abstract: Saxitoxin (STX) and some selected paralytic shellfish poisoning (PSP) analogues in mussel samples were identified and quantified with liquid chromatography-tandem mass spectrometry (LC-MS/MS). Sample extraction and purification methods of mussel sample were optimized for LC-MS/MS analysis. The developed method was applied to the analysis of the homogenized mussel samples in the proficiency test (PT) within the EQuATox project (Establishment of Quality Assurance for the Detection of Biological Toxins of Potential Bioterrorism Risk). Ten laboratories from eight countries participated in the STX PT. Identification of PSP toxins in naturally contaminated mussel samples was performed by comparison of product ion spectra and retention times with those of reference standards. The quantitative results were obtained with LC-MS/MS by spiking reference standards in toxic mussel extracts. The results were within the z-score of ±1 when compared to the results measured with the official AOAC (Association of Official Analytical Chemists) method 2005.06, pre-column oxidation high-performance liquid chromatography with fluorescence detection (HPLC-FLD).
authors.affiliation: VERIFIN (Finnish Institute for Verification of the Chemical Weapons Convention), Department of Chemistry, University of Helsinki, P.O. Box 55, A. I. Virtasen aukio 1 FI-00014, Finland. kirsi.harju@helsinki.fi.
authors.forename: Kirsi
authors.initials: K
authors.lastname: Harju
authors.affiliation: VERIFIN (Finnish Institute for Verification of the Chemical Weapons Convention), Department of Chemistry, University of Helsinki, P.O. Box 55, A. I. Virtasen aukio 1 FI-00014, Finland. marja-leena.rapinoja@helsinki.fi.
authors.forename: Marja-Leena
authors.initials: ML
authors.lastname: Rapinoja
authors.affiliation: Federal Department of Defence, Civil Protection and Sport, SPIEZ LABORATORY, Austrasse 1, Spiez CH-3700, Switzerland. marc-andre.avondet@babs.admin.ch.
authors.forename: Marc-André
authors.initials: MA
authors.lastname: Avondet
authors.affiliation: Federal Department of Defence, Civil Protection and Sport, SPIEZ LABORATORY, Austrasse 1, Spiez CH-3700, Switzerland. werner.arnold@babs.admin.ch.
authors.forename: Werner
authors.initials: W
authors.lastname: Arnold
authors.affiliation: Federal Department of Defence, Civil Protection and Sport, SPIEZ LABORATORY, Austrasse 1, Spiez CH-3700, Switzerland. martin.schaer@babs.admin.ch.
authors.forename: Martin
authors.initials: M
authors.lastname: Schär
authors.affiliation: Marine Institute, Marine Environment and Food Safety Services, Rinville, Oranmore, Co. Galway, Ireland. stephen.burrell@marine.ie.
authors.forename: Stephen
authors.initials: S
authors.lastname: Burrell
authors.affiliation: ChemStat, Aarstrasse 98, Bern CH-3005, Switzerland. info@chemstat.ch.
authors.forename: Werner
authors.initials: W
authors.lastname: Luginbühl
authors.affiliation: VERIFIN (Finnish Institute for Verification of the Chemical Weapons Convention), Department of Chemistry, University of Helsinki, P.O. Box 55, A. I. Virtasen aukio 1 FI-00014, Finland. paula.vanninen@helsinki.fi.
authors.forename: Paula
authors.initials: P
authors.lastname: Vanninen
mesh_terms: D000818:Animals; D002853:Chromatography, Liquid; D059021:Laboratory Proficiency Testing; D008387:Marine Toxins / Q000032:analysis*; D049878:Mytilus; D057096:Shellfish Poisoning; D053719:Tandem Mass Spectrometry
chemical_list: D008387:Marine Toxins
keywords: liquid chromatography-mass spectrometry; mussel; paralytic shellfish poisoning toxins; saxitoxin