T3-01 Enabling Accurate Measurements of Staphylococcal Enterotoxin A (SEA) in Food by Use of a Comprehensively Characterised Calibrant Solution

Wednesday, 29 March 2017: 16:00
314-316 (The Square)
Reinhard Zeleny, European Commission, Geel, Belgium
Sébastien Boulo, European Commission, Geel, Belgium
Amalia Muñoz, European Commission, Geel, Belgium
Heinz Schimmel, European Commission, Geel, Belgium
Dominique Baiwir, University of Liège, Liège, Belgium
Gabriel Mazzucchelli, University of Liège, Liège, Belgium
Isabelle Mutel, Université Paris-Est, ANSES, Laboratory for Food Safety, Maisons-Alfort, France
Yacine Nia, Université Paris-Est, ANSES, Maisons-Alfort, France
Introduction:  Staphylococcal enterotoxins account for a substantial number of food poisoning outbreaks in the EU and elsewhere. Besides the current methods, which are mainly focussed on presence/absence testing (toxin detected/not-detected), more and more quantitative methods are being developed (e.g. immunochemical assays, mass spectrometry-based methods). For accurate quantification of toxin levels in complex food matrices, however, suitable calibration solutions are required.

Purpose:  The scope of the study was an in-depth purity and identity characterisation of commercially available Staphylococcal enterotoxin A (SEA) and the accurate determination of the protein concentration of a solution prepared from the lyophilised toxin, with the aim to produce a suitable calibration solution for quantitative SEA measurements.

Methods:  The set of methods applied to assess the purity and identity of the toxin comprised of SDS-PAGE (initial mass determination), Q-TOF (accurate mass determination), multi-enzyme LC-MS/MS (sequencing of the protein for identity), and ELISA (cross-reactivity check and indicative concentration). The prepared SEA stock solution was value assigned for its protein concentration by amino acid analysis (AAA), using an in-house isotope dilution LC-MS/MS method.

Results:  SDS-PAGE indicated one major band, confirming the >95% purity statement issued by the material provider. Sequencing confirmed the published SEA sequence, and ELISA for Staphylococcal enterotoxins A-D confirmed the absence of those toxins in the preparation. However, a strong cross-reaction was obtained with a SEE-specific ELISA (sequence similarity of SEA and SEE). AAA provided a reliable means to establish the protein concentration of the SEA solution. Moreover, AAA measurements spread over a period of 3 years confirmed excellent sample stability for a storage at -20⁰C.

Significance:  The comprehensively characterised and thoroughly value-assigned SEA solution provides the basis for accurate quantitative SEA analyses in complex food matrices; and thus, will contribute to establish and maintain reliable measurement results for effective consumer protection.