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Results of a Saxitoxin Proficiency Test Including Characterization of Reference Material and Stability Studies
 
 
Article

Optimization of Sample Preparation for the Identification and Quantification of Saxitoxin in Proficiency Test Mussel Sample using Liquid Chromatography-Tandem Mass Spectrometry

1
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
2
Federal Department of Defence, Civil Protection and Sport, SPIEZ LABORATORY, Austrasse 1, Spiez CH-3700, Switzerland
3
Marine Institute, Marine Environment and Food Safety Services, Rinville, Oranmore, Co. Galway, Ireland
4
ChemStat, Aarstrasse 98, Bern CH-3005, Switzerland
*
Author to whom correspondence should be addressed.
Academic Editor: Andreas Rummel
Toxins 2015, 7(12), 4868-4880; https://doi.org/10.3390/toxins7124853
Received: 18 June 2015 / Revised: 30 July 2015 / Accepted: 4 August 2015 / Published: 25 November 2015
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). View Full-Text
Keywords: paralytic shellfish poisoning toxins; saxitoxin; liquid chromatography-mass spectrometry; mussel paralytic shellfish poisoning toxins; saxitoxin; liquid chromatography-mass spectrometry; mussel
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MDPI and ACS Style

Harju, K.; Rapinoja, M.-L.; Avondet, M.-A.; Arnold, W.; Schär, M.; Burrell, S.; Luginbühl, W.; Vanninen, P. Optimization of Sample Preparation for the Identification and Quantification of Saxitoxin in Proficiency Test Mussel Sample using Liquid Chromatography-Tandem Mass Spectrometry. Toxins 2015, 7, 4868-4880. https://doi.org/10.3390/toxins7124853

AMA Style

Harju K, Rapinoja M-L, Avondet M-A, Arnold W, Schär M, Burrell S, Luginbühl W, Vanninen P. Optimization of Sample Preparation for the Identification and Quantification of Saxitoxin in Proficiency Test Mussel Sample using Liquid Chromatography-Tandem Mass Spectrometry. Toxins. 2015; 7(12):4868-4880. https://doi.org/10.3390/toxins7124853

Chicago/Turabian Style

Harju, Kirsi, Marja-Leena Rapinoja, Marc-André Avondet, Werner Arnold, Martin Schär, Stephen Burrell, Werner Luginbühl, and Paula Vanninen. 2015. "Optimization of Sample Preparation for the Identification and Quantification of Saxitoxin in Proficiency Test Mussel Sample using Liquid Chromatography-Tandem Mass Spectrometry" Toxins 7, no. 12: 4868-4880. https://doi.org/10.3390/toxins7124853

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