Optimization of Sample Preparation for the Identification and Quantification of Saxitoxin in Proficiency Test Mussel Sample using Liquid Chromatography-Tandem Mass Spectrometry
Kirsi Harju,
Marja-Leena Rapinoja,
Marc-André Avondet,
Werner Arnold,
Martin Schär,
Stephen Burrell,
Werner Luginbühl,
Paula Vanninen
Affiliations
Kirsi Harju
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
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
Marc-André Avondet
Federal Department of Defence, Civil Protection and Sport, SPIEZ LABORATORY, Austrasse 1, Spiez CH-3700, Switzerland
Werner Arnold
Federal Department of Defence, Civil Protection and Sport, SPIEZ LABORATORY, Austrasse 1, Spiez CH-3700, Switzerland
Martin Schär
Federal Department of Defence, Civil Protection and Sport, SPIEZ LABORATORY, Austrasse 1, Spiez CH-3700, Switzerland
Stephen Burrell
Marine Institute, Marine Environment and Food Safety Services, Rinville, Oranmore, Co. Galway, Ireland
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
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).
